Pectin
Pectin
Original article
Resistance of industrial mango peel waste to pectin degradation
prior to by-product drying
Summary            Susceptibility of industrial mango peel waste to pectin degradation during storage at ambient conditions
                   (25 C, 63% relative humidity) for up to 5 h before by-product stabilisation by drying was explored.
                   Depending on the interim storage period in the wet state, pectins were recovered from the dried peels by hot-
                   acid extraction. Most important, pectin degradation during the temporary storage of the wet peels was
                   insignificant, as revealed by yields, composition, average molecular properties, and techno-functional
                   quality. Hardly acetylated (DAc 2.5–4.5%), rapid-set high-methoxyl pectins were obtained at starch-
                   corrected net yields of 14.1–15.6 g hg)1. Irrelevant de-esterification during peel storage in the wet state was
                   confirmed by overall uniform setting temperatures. Arabinogalactans, uniformly indicated by high molar
                   galactose ⁄ rhamnose ratios of 13.8–16.9 mol ⁄ mol and an arabinose percentage of 9.5–14.4 mol hmol)1 of
                   galactose residues, affected the galacturonide contents, intrinsic viscosities, and gel strengths throughout.
                   The wet peels, derived from widespread manual peeling in mango canning, tolerated intermediate storage for
                   5 h, thus facilitating by-product stabilisation on smaller scales.
Keywords           By-product drying, enzymatic degradation, fruit processing, intermediate storage, mango (Mangifera indica L.), pectin, waste
                   utilisation.
doi:10.1111/j.1365-2621.2010.02314.x
 2010 The Authors. Journal compilation  2010 Institute of Food Science and Technology
1648   Stability of mango peel by-products S. Sirisakulwat et al.
       through endo- (EC 3.2.1.15) and exo-acting (EC 3.2.               As regards a secure and economic supply of high-
       1.67) polygalacturonases (PG), pectin methyl esterases         quality mango by-products for further upgrading, this
       (PME, EC 3.1.1.11) affecting the degree of esterification        study therefore aimed at evaluating the proneness of
       are most crucial. Without immediate drying or at least         industrial peel waste to pectin degradation during a
       blanching of citrus peels, even slight de-esterification        temporary dwell time at ambient conditions until
       because of high endogenous PME activities may cause            drying. The tolerable period between waste production
       calcium-sensitive pectins unsuitable as gelling agents         (peeling) and drying was to be identified, mimicking
       (Voragen et al., 1995). Apart from some soluble forms,         different operational situations in mango processing.
       PME is mainly associated with cell wall proteins by            The contribution of by-product handling to the varia-
       ionic interactions (Benen et al., 2003a). Additionally,        tions of mango pectins in yield and quality was to be
       pectin homogalacturonan acetylesterases (PAE, EC 3.1.          assessed.
       1.6) occur in orange and a few other plant species
       (Benen et al., 2003a). Aside from PG, pectate lyase
                                                                      Materials and methods
       (PAL, EC 4.2.2.2) and endo-rhamnogalacturonan
       hydrolase (endoRGH) have been found in plants as
                                                                      Sample material and experimental design
       further pectin backbone depolymerases (Benen et al.,
       2003b). Degradation of pectin side chains involves             Industrial peel waste, originating from ‘Kaew Khiew’
       arabinanases and galactanases, such as a carrot                mango fruit, was obtained from a canning factory in
       a-l-arabinofuranosidase (EC 3.2.1.55) and a tomato             Chiang Mai, Thailand, during the mango processing
       exo-b(1 fi 4)-d-galactanase (De Vries & Visser, 2003).          campaign in April 2005. Nine samples were consecu-
       During fruit ripening, plant b-d-galactosidases (EC            tively drawn within 4 h. For each of them, 1800 g of
       3.2.1.23), increasing in parallel with tissue softening,       fresh peel waste was quickly collected from three manual
       cause pectin depolymerisation by side-chain loss and           peeling lines by randomly picking the material from
       enhanced pectin solubilisation (Brummell, 2006). In            various positions of the lines directly after its removal
       ripening mango mesocarp, b-d-galactosidase activity            from the fruit. To explore the tolerable period between
       even rose to the eightfold level from the mature-green         peeling and waste drying, the peels of each sample were
       to the ripe stage, but PG and b(1 fi 4)-d-glucanase             exposed to the ambient conditions of the peeling room
       (EC 3.2.1.4) only to the 1.6- and 2.4-fold activities,         (25 C; 63% relative humidity, RH) in an open bowl
       while PME declined to 41% (Ali et al., 2004).                  for holding times (HT25 C) of 0 (variant MPW1),
       Although the mango cultivars may differ in the                  15 (MPW2), 30 (MPW3), 60 (MPW4), 90 (MPW5),
       properties of three PG isoforms (Prasanna et al.,              120 (MPW6), 180 (MPW7), 240 (MPW8), and 300 min
       2006; Singh & Dwivedi, 2008), mango PG turned out              (MPW9), respectively. Subsequently, the peels of each
       to be mainly exo-acting (Ali et al., 2004). Homogalac-         sample were packed as a thin layer into a polyethylene
       turonan degradation in mango mesocarp has thus                 (PE) pouch and frozen in a freezer, which was tempo-
       recently been ascribed to a softening-related PAL              rarily installed near the peeling lines. So far, the
       rather than to PG (Chourasia et al., 2006). Consistent         experiment was performed close to the peeling lines
       with much lower, rather constant PME and PG                    when they were in full operation. Because of limited
       activities in the peel relative to the mesocarp (Yanru         drying capacity, the samples were temporarily stored at
       et al., 1995), carbohydrate changes in mango peels             )20 C until drying. Without previous external thawing,
       because of postharvest ripening were mainly restricted         the frozen peel samples were dried at 80 C for approx-
       to the degradation of starch and matrix glycan frag-           imately 4 h in a fluidized-bed laboratory dryer (Rapid
       ments (Sirisakulwat et al., 2008).                             dryer TG 1, Retsch, Haan, Germany) until a moisture
          On the other hand, the mango fruit may predomi-             content of 4.5–6.6 g hg)1. After weighing to record the
       nantly be processed at higher ambient temperature and          yield of the dried mango peel waste (MPW)
       humidity than the citrus fruit and apples in view of the       (21.6–29.8 g hg)1 of fresh peel waste), the dried peels
       climate in the respective growing areas. Therefore,            were vacuum-packed into PE pouches and transported
       rather adverse conditions during a temporary storage           by airfreight to Hohenheim University, Stuttgart,
       of wet mango peels between peeling and by-product              Germany, where they were manually crushed, vacuum-
       drying may occur in practice. Their impact on pectin           packed into PE pouches, and stored at ambient temper-
       quality must be known with respect to minimum                  ature (approximately 22–25 C) in a desiccator until
       requirements for sustainable by-product stabilisation          pectin extraction. By using the methodology detailed
       processes when evaluating this potential raw material          earlier (Sirisakulwat et al., 2008), the recovered pectins
       source, primarily because mango processing represents a        were characterised in terms of composition as well as
       very multifaceted field with a wide range of production         average molecular and techno-functional properties.
       scales (Vásquez-Caicedo et al., 2004, 2007; Pott et al.,      Analytical and empirical methods commonly used by
       2005).                                                         pectin producers for quality assessment were included.
       International Journal of Food Science and Technology 2010     2010 The Authors. Journal compilation  2010 Institute of Food Science and Technology
                                                                                                     Stability of mango peel by-products S. Sirisakulwat et al.   1649
   Ripeness of the fruit processed was assessed at                                        Darmstadt, Germany). The ground AIS was subjected
Chiang Mai University, Chiang Mai, Thailand, by                                           to pectin characterisation.
analogy to a previous study (Sirisakulwat et al., 2008)
on the basis of five fruits that were randomly selected
                                                                                          Chemical pectin characterisation
among the fruits provided for peeling. The maturity-
specific properties of the edible part included the pH                                     The AIS composition was analysed as detailed previ-
value (pH 3.85 ± 0.01) and the contents of total                                          ously (Sirisakulwat et al., 2008). In brief, the galacturo-
soluble solids (TSS; 18.7 ± 0.07 Brix) and titratable                                    nide content was titrimetrically quantified in duplicate
acids (TA as citric acid, pH 8.1; 0.58 ± 0.01 g hg)1),                                    from the neutralisation and saponification equiva-
corresponding to a sugar ⁄ acid ratio (TSS ⁄ TA) of                                       lents and expressed as galacturonic acid (Mr =
32.2 ± 0.7. Mesocarp firmness, measured with an                                            194.1 g mol)1) on an ash- and moisture-free basis
Instron Universal Texture Analyzer type 3365 (Instron,                                    [GalUAtitr, g hg)1 of purified AIS (AISp)] according to
Canton, MA, USA) as specific maximum load (SFKS)                                           the legal pectin specification (Joint FAO ⁄ WHO Expert
by using a Kramer shear cell (Vásquez-Caicedo et al.,                                    Committee on Food Additives (JECFA), 2007). Based
2006), ranged at 472 ± 9 N hg)1. Compared to the                                          on the recovery rate after AIS purification in acidified
mango fruit of a related study (Sirisakulwat et al.,                                      propan-2-ol (AISp ⁄ AIS, g g)1), GalUAtitr was converted
2008), the mesocarp properties came overall most close                                    into the anhydrogalacturonic acid content of the
to those of the ‘Kaew Khiew’ (KAk) batch, which had                                       original sample (AUAtitr, g hg)1 of AIS; Mr =
previously been examined after major fruit softening                                      176.13 g mol)1). By analogy, its methylester content
(ripeness stage II). For this batch, a TSS ⁄ TA ratio of                                  (Mr = 31 g mol)1) was calculated (MeOHtitr, g hg)1 of
55.2 ± 0.9 was reported. Its mesocarp firmness of                                          AIS) from the saponification equivalents. The degree of
4.4 ± 0.1 N, recorded with a Warner–Bratzler shear                                        esterification (DE) resulted as the percentage of the
cell, corresponded to a SFKS of 519 ± 19 N hg)1                                           saponification equivalents relative to the total of neu-
measured concomitantly. For comparison, full-ripe                                         tralisation and saponification equivalents. After acid
fruit (stage III) had then been characterised by a                                        hydrolysis of the AIS using H2SO4 (72% w ⁄ w) at
TSS ⁄ TA ratio of 94.1 ± 2.6 and low firmness records                                      ambient temperature, the anhydrouronic acid content
of 1.8 ± 0.04 N and 373 ± 12 N hg)1, respectively                                         (Mr = 176.13 g mol)1) was additionally quantified col-
(Sirisakulwat et al., 2008). Compared to these two                                        orimetrically (AUAc, g hg)1 of AIS) in triplicate with
batches, the fruit of this study thus had a lower sugar                                   m-hydroxydiphenyl in photometric series analyses. The
content and TSS ⁄ TA ratio, but mesocarp firmness was                                      absorbance was measured at 520 nm against a sample
intermediate.                                                                             blank with a Cary 100 spectrophotometer (Varian,
                                                                                          Mulgrave, VIC, Australia).
                                                                                             The neutral sugars were determined in duplicate
Pectin extraction from dried mango peel waste
                                                                                          as their alditol acetates by gas chromatography (GC)
Industrial hot-acid extraction was mimicked on a                                          with flame ionisation detection after acid hydrolysis
laboratory scale. Pectin was extracted from the dried                                     (Sirisakulwat et al., 2008). After prehydrolysis at ambi-
raw material (DRM) at pH 1.5, applying a standard                                         ent temperature (60 min) using H2SO4 (72% w ⁄ w), the
protocol (Sirisakulwat et al., 2008) to the dried MPW                                     AIS samples were diluted with N2-saturated, ultra-pure
on the double scale throughout. Per run, 40 g of MPW                                      water and subjected to hot-acid hydrolysis (121 C, 1 h)
was filled up with distilled water to a total of 800 g. The                                in an electric heating block. The neutral sugars were
suspension was boiled for 15–20 min and recooled. The                                     reduced with sodium borohydride, followed by acetyla-
pH was adjusted to 1.5 with H2SO4 (25% w ⁄ w) prior to                                    tion of the alditols with acetic anhydride in the presence
extraction (90 C, 2.5 h) in an oil bath. Separation of the                               of 1-methyl imidazole as catalyst. For GC analyses, the
extract as well as precipitation in propan-2-ol (‡ 99.9%                                  alditol acetates were extracted from the aqueous phase
v ⁄ v) and drying (60 C, 1–2 h) of the pectins were                                      with ethyl acetate, produced after the addition of
performed as described previously (Sirisakulwat et al.,                                   absolute ethanol. Myo-inositol was used as internal
2008). Nine runs were carried out for each MPW                                            standard.
sample. For each run, the yield of dried crude pectin was                                    Based on the simultaneous HPLC analysis of meth-
calculated as alcohol-insoluble substance (AIS, g hg)1 of                                 anol (MeOH, Mr = 32.04 g mol)1) and acetic acid
DRM). Per sample, the AIS of all runs was pooled and                                      (Mr = 60.05 g mol)1) after saponification in alkaline
ground in a centrifugal mill type ZM 1 (Retsch, Haan,                                     propan-2-ol, the degrees of methylation (DMe) and
Germany) to particle sizes <0.25 mm. The starch-                                          acetylation (DAc) were calculated as the respective
corrected pectin yield (AISS-corr, g hg)1 of DRM) was                                     molar ratios to AUAc (Sirisakulwat et al., 2008). The
calculated (Sirisakulwat et al., 2008) after enzymatic                                    methanol and acetyl contents (g hg)1 of AIS) were
quantification of co-extracted starch (g hg)1 of AIS) by                                   quantified by using the 2695 Separations Module of a
means of the respective test combination (R-Biopharm,                                     Waters HPLC Alliance system (Waters, Milford, MA,
 2010 The Authors. Journal compilation  2010 Institute of Food Science and Technology             International Journal of Food Science and Technology 2010
1650   Stability of mango peel by-products S. Sirisakulwat et al.
       USA) with a Waters 2410 refractive index detector set to         buffer (0.25 mol kg)1 of gel), the setting temperatures
       35 C. An Aminex HPX-87H column (300 · 7.8 mm;                   were assayed by dynamic rheometric analyses in dupli-
       Bio-Rad Laboratories, Hercules, CA, USA) was eluted              cate or triplicate, using a Bohlin CVO 120 HR rheom-
       at 40 C with 0.01 n H2SO4 (0.6 mL min)1). Samples               eter (Malvern Intruments, Herrenberg, Germany) with a
       were prepared in duplicate with two injections per vial.         Searle cylinder device (C 25) (Sirisakulwat et al., 2008).
       Lithium lactate, dissolved in alkaline propan-2-ol,              The AIS, premixed with a small portion of the sucrose,
       served as internal standard.                                     was carefully dispersed at ambient temperature in the
          The moisture content (g hg)1 of AIS) was gravimet-            diluted buffer that resulted from 68 g of distilled water
       rically determined in duplicate as mass loss after drying        and 17 g of a KOAc ⁄ HOLc buffer stock solution
       of 1 g of AIS in a porcelain crucible at 105 ± 2 C in a         [KOAc: 40.48 g L)1; HOLc (90%): 188.05 g L)1]. When
       hot-air cabinet for 2 h (Joint FAO ⁄ WHO Expert                  the AIS was completely dissolved under heating in
       Committee on Food Additives (JECFA), 2007) and                   the presence of 1–2 drops of defoaming emulsion, the
       recooling in a desiccator until constant weight. After           remaining part of the sugar was stepwise added to the
       slow preincineration of the moisture-free AIS on an              boiling mixture. TSS was adjusted by cooking to a
       electric heating plate, the ash content (g hg)1 of AIS)          precalculated net weight of 170 g under stirring. Subse-
       was quantified by complete incineration (550 C, 3 and            quently, the sample was poured into the preheated C 25
       16 h) in a muffle furnace with intermediate wetting of             device (90 C). To avoid evaporation and superficial
       the recooled sample [2–4 drops of ultra-pure water and           hardening, the free sample surface was covered with hot
       4–5 drops of H2O2 (30% w ⁄ w)] and drying (105 ± 2 C,           low-viscous liquid paraffin. Gel formation was moni-
       1 h) (Sirisakulwat et al., 2008). The mass of the white          tored by measuring the storage (G¢) and the loss (G¢¢)
       ash was verified after further incineration (550 C, 1 h)         moduli as well as the phase angle [d = arctan (G¢¢ ⁄ G¢)]
       and recooling (60 min).                                          at a fixed frequency (f = 1 Hz) and strain amplitude
                                                                        (c = 0.015) as a function of time (t, s) during cooling
                                                                        from 90 to 20 C at a constant rate (DT = )0.999 ±
       Quantification of average macromolecular pectin properties
                                                                        0.002 K min)1). In the sol–gel transition range, the d-t
       The intrinsic viscosity ([g], mL g)1) was assessed as an         curves were iteratively approximated by a modified
       average parameter influenced by all polymers of an AIS            logistic four-parameter model (Neidhart et al., 2003),
       sample. Based on the single-point relationship (Solo-            using the NLIN procedure (Marquardt method) of the
       mon-Ciuta equation), it was computed from the specific            Statistical Analysis System (SAS) 9.1 (SAS Institute,
       viscosities [gsp ¼ ðgs  go Þ=go ] of different AIS solutions     Cary, NC, USA). The setting time (td¼45 , s) and
       as a mean of ten records and verified by the Huggins              temperature (Td¼45 , C) were deduced from the cross-
       plot and the Kraemer plot as detailed previously                 over-point of the moduli [d(1 Hz) = 45].
       (Sirisakulwat et al., 2008). The AIS contents (c) of five            The gel properties were characterised by the breaking
       solutions per sample were adjusted to the gsp range of           strengths (BS) of pectin-sucrose gels (TSS = 65 Brix,
       0.2–1 (Morris, 1995) by appropriate dilution of a sample         pH 3) with AIS doses of 0.3 and 0.35 g hg)1 in a
       stock solution (c = 0.3–0.4 g dL)1) with the solvent.            KOAc ⁄ HOLc buffer (0.28 mol kg)1 of gel) on the basis
       The dynamic viscosities (g = Kqt, mPa s) of AIS                  of an empirical tension test established for the stan-
       solutions (gs) and solvent (go) were calculated from the         dardisation of pectins and the comparative evaluation of
       flow time (t, s), measured at 20 C for a test volume of          pectin sources (Endress & Dilger, 1990). By using the
       2 mL (2 · 3 runs for to and ts, respectively) by using a         Herbstreith-Pectinometer type Mark III (Herbstreith &
       Micro-Ostwald capillary viscosimeter (capillary con-             Fox, Neuenbürg, Germany), the BS was recorded in
       stant K = 0.01181 mm2 s)2). The densities (q, g cm)3)            device-specific units (Herbstreith-Pectinometer units,
       of AIS solutions (qs) and solvent (qo) were measured at          HPE). The AIS dose required for a standardised gel
       20 C with a density meter DMA 48 (Anton Paar, Graz,             (BS = 530 HPE) was calculated by interpolation as the
       Austria). The AIS was dissolved under automatic                  breaking capacity of the AIS (BC530HPE, g hg)1 of gel).
       shaking (16 h) before adjusting the volume of the stock          By dividing the sugar content of this gel (TSS) by
       solution to 100 mL. A 0.28 m buffer (pH 3.0 ± 0.05) of            BC530HPE, the gelling capacity of the AIS (SBC530HPE,
       potassium acetate (KOAc: 4.57 g L)1) and lactic acid             g g)1 of AIS) was obtained as the sugar-binding
       [HOLc (90%): 23.59 g L)1] served as solvent, mimicking           capacity, i.e., the amount of sugar bound by this AIS
       the gel systems used for the gelation studies in terms of        dose in a gel of 530 HPE. Multiplication of SBC530HPE
       pH and concentration.                                            with the AIS content of the DRM (dried MPW) yielded
                                                                        the corresponding gelling capacity of the DRM
                                                                        extracted (SBCDRM, g hg)1 of DRM). With each AIS
       Characterisation of techno-functional pectin properties
                                                                        dose, a gel was prepared by cooking the AIS-containing
       For pectin-sucrose gels (TSS = 65 Brix, pH 3) with              mixture on the basis of 216.0 g of sugar and 147.0 g of a
       AIS doses (cp) of 0.4 and 0.55 g hg)1 in a KOAc ⁄ HOLc           0.65 m KOAc ⁄ HOLc buffer [KOAc: 10.5 g L)1; HOLc
       International Journal of Food Science and Technology 2010       2010 The Authors. Journal compilation  2010 Institute of Food Science and Technology
                                                                                                                      Stability of mango peel by-products S. Sirisakulwat et al.                                                                1651
MPW 9
MPW 1
                                                                                                                                         MPW 8
experimentally verified. For their normalisation to
                                                                                                                                                 MPW 7
                                                                                                                                                 MPW 6
MPW 2
MPW 4
                                                                                                                                                                                             MPW 3
                                                                                                            450
                                                                                                                                                                    MPW 5
                                                                                                                                                                                                           20
constant AUA levels, BC530HPE and SBC530HPE were                                                            400
related to the AUAtitr content of the AIS and expressed                                                                                                                                                    15
                                                                                                            350
as BC530HPE (AUAtitr) [in g of AUA hg)1 of gel] and                                                                                                                                                        10
                                                                                                            300
SBC530HPE (AUAtitr) [in g of sugar g)1 of AUA],
                                                                                                            250                                                         5
respectively.                                                                                                     0     60         120         180        240        300
                                                                                                                  MPW Sampling relative to the first sampling point (min)
                                                                                                            Intrinsic viscosity                          Gal/Rha               AUA c /Rha            AUA titr /Rha
Results and discussion
                                                                                          Figure 1 Variability of peel quality throughout by-product sampling
Impact of peel storage on pectin yields                                                   for variants MPW1-MPW9: Intrinsic viscosities ([g]) as well as molar
                                                                                          ratios of galactose to rhamnose (Gal ⁄ Rha) and colorimetric or
Irrespective of the exposure of the wet peels to the                                      titrimetric anhydrogalacturonic acid to rhamnose (AUAc ⁄ Rha,
ambient conditions of the peeling room (25 C; 63%                                        AUAtitr ⁄ Rha) of the alcohol-insoluble substance extracted from
RH) for up to 5 h, the crude pectin yields (AIS) from                                     dried peel waste (MPW) that accrued from the industrial canning of
hot-acid extraction of the dried by-products amounted                                     ‘Kaew Khiew’ mango fruit after exposure of the wet peels to the
to 14.7–16.2 g hg)1 of DRM, with the median ranging                                       ambient conditions of the peeling room (25 C, 63% relative humidity)
at 15.7 g hg)1 (Table 1). Because of comparatively low                                    for different holding times (variants MPW1-MPW9; cf. Table 1)
starch contents of 2.2–5.6 g hg)1 of AIS, the net pectin                                  prior to waste stabilisation. For each variant, the time of sampling is
yields (AISS-corr) were 14.1–15.6 g hg)1 of DRM. The                                      expressed on the abscissa relative to that of variant MPW9, which
                                                                                          was collected first.
chronological order of peel sampling is exemplarily
shown in Fig. 1. As revealed by respective sorting of the
samples, the highest crude and net pectin yields were                                        Industrial hot-acid extraction in pectin recovery from
uniformly recorded for the first (MPW9) and the last                                       established sources (MacDougall & Ring, 2004) was
sample (MPW3), whereas the largest differences were                                        mimicked by the procedure applied on the laboratory
observed for the three samples collected within the first                                  scale. With a median of 15.2 g hg)1 of DRM, the net
64 min (MPW9, MPW1, and MPW8). Moreover, the                                              pectin yields of the samples roughly matched the
peel sample dried without previous dwell period at                                        average reported for hot-acid extraction of dried mango
ambient temperature (MPW1) was among those show-                                          peels (Neidhart et al., 2009), slightly exceeding the
ing the lowest net pectin yield, whereas MPW9 peaked                                      pectin amounts extracted with the same method from
despite the interim storage of the wet peels for 5 h. Thus,                               peels of the same cultivar (‘Kaew Khiew’, KAk; 12.9–
the temporary exposure of the residues to the ambient                                     13.1 g hg)1) when the impact of cultivar and fruit
conditions of the peeling room did not affect the                                          ripeness was studied (Sirisakulwat et al., 2008). Findings
achievable pectin yields. In fact, it was the natural                                     detailed elsewhere for peels of related and other mango
heterogeneity of the peel waste that was reflected by the                                  cultivars (Berardini et al., 2005a,b; Koubala et al., 2008)
observed yield variations.                                                                were concordant with the median net pectin yield
Table 1 Yields of alcohol-insoluble substance (AIS) extracted from dried peel waste (MPW) that accrued from the industrial canning of
‘Kaew Khiew’ mango fruit after exposure of the wet peels to the ambient conditions of the peeling room (25 C, 63% relative humidity) for
different holding times (HT25 C) up to 5 h prior to waste stabilisation
Variant MPW1 MPW2 MPW3 MPW4 MPW5 MPW6 MPW7 MPW8 MPW9
AISa (g hg)1 DRM)              14.9 ± 0.1      15.6 ± 0.2      16.2 ± 0.2       15.7 ± 0.2            15.8 ± 0.2                   15.5 ± 0.3                     15.7 ± 0.1      14.7 ± 0.3         16.2 ± 0.1
Starchb (g hg)1 AIS)            5.6 ± 0.1       4.0 ± 0.2       3.7 ± 0.02       3.0 ± 0.1             4.2 ± 0.2                    2.2 ± 0.03                     3.6 ± 0.2       3.9 ± 0.2          3.8 ± 0.002
AISS-corrc (g hg)1 DRM)        14.1 ± 0.1      14.9 ± 0.2      15.6 ± 0.2       15.3 ± 0.2            15.1 ± 0.2                   15.2 ± 0.3                     15.2 ± 0.1      14.1 ± 0.3         15.6 ± 0.1
 2010 The Authors. Journal compilation  2010 Institute of Food Science and Technology                           International Journal of Food Science and Technology 2010
1652   Stability of mango peel by-products S. Sirisakulwat et al.
       mentioned above. At last, the mango peels were quite                                      experimental full-ripe fruit batch of the same cultivar
       similar to apple pomace in terms of AIS yields (Endress                                   (specified as cv. ‘Kaew Khiew’ at ripeness stage III;
       et al., 2006).                                                                            Sirisakulwat et al., 2008). Similarities between this
          However, in wet mango peels, the pectic substances                                     sample and the nine pectins from industrial peel waste
       obviously degraded less readily compared to wet apple                                     were furthermore observed in terms of the total neutral
       pomace, although the mango fruit may predominantly                                        sugars (ANS, 35.9 ± 0.1 vs. 31–36 g hg)1) as well as the
       be processed at higher ambient temperature and humid-                                     titrimetrically quantified anhydrogalacturonic acid
       ity. Unlike apple pomace, MPW usually accrues with far                                    (AUAtitr, 34.7 ± 0.1 vs. 38–42 g hg)1) and methylester
       less tissue disintegration. In manual peeling, which is                                   contents (MeOHtitr, 4.38 ± 0.02 vs. 4.7–5.2 g hg)1).
       still usual practice in many canning and drying factories,                                The slightly higher values of the latter nine samples
       thick peel strips accumulate. Therefore, cell de-com-                                     (Table 2) might largely be ascribed to improved purity,
       partmentalisation is restricted to the thin cutting edges                                 which became evident in lower ash contents (16.2 ± 0.2
       and the mesocarp-facing cut surface. Consistently, cold                                   vs. 8–10 g hg)1) at comparable moisture levels (4.3 ±
       storage (2 ± 1 C) of fresh and blanched MPW (mois-                                       0.1 vs. 4.9–5.7 g hg)1). However, it should be noted
       ture content: 85–89%) for 3 and 6 days, respectively,                                     that, unlike the previous study (Sirisakulwat et al.,
       was considered tolerable without loss of pectin yield                                     2008), mass balances of 90–93% [total (2), Table 2],
       (Sudhakar & Maini, 2000), but pectin quality was not                                      resulting from the total neutral sugars, both titrimetri-
       evaluated in this context.                                                                cally analysed parameters, ash, and moisture, indicated
                                                                                                 slight underestimation of the composition for the nine
                                                                                                 AIS samples. Proteins reported for acid-extracted
       Impact of peel storage on pectin structure
                                                                                                 mango peel pectins might contribute further 1.1–3.3%
       Like the yield, also the overall composition of the                                       (Kratchanova et al., 1991). Whereas the AUAtitr and
       pectins was apparently unaffected by the exposure of                                       MeOHtitr contents were expected to be confirmed by
       the wet mango peels to the ambient conditions of the                                      further methods applied (Sirisakulwat et al., 2008), the
       peeling room for up to 5 h (Table 2). With 4.8 ±                                          colorimetric anhydrogalacturonic acid contents of
       0.2 g hg)1 of AIS, a low starch content within the limits                                 the nine samples (AUAc, 49–58 g hg)1) systematically
       observed for the nine AIS samples (Table 1) was                                           exceeded the titrimetric values (AUAtitr) by approxi-
       previously reported for the pectin, which had been                                        mately 12 g hg)1 on average, the methoxyl contents
       extracted in the same way (pH 1.5) from the peels of an                                   resulting from methanol analysis by HPLC (MeOH,
       Table 2 Composition of the alcohol-insoluble substance (AIS) extracted from dried peel waste (MPW) that accrued from the industrial canning of
       ‘Kaew Khiew’ mango fruit after exposure of the wet peels to the ambient conditions of the peeling room (25 C, 63 % relative humidity) for
       different holding times (HT25 C) up to 5 h prior to waste stabilisation: Mass balancea
Variant MPW1 MPW2 MPW3 MPW4 MPW5 MPW6 MPW7 MPW8 MPW9
       Moisture             5.7 ±     0.1     4.9 ±   0.1     5.1 ±   0.1      5.3 ±   0.03        5.5 ±   0.01       5.5 ±   0.04     5.3 ±   0.1      5.5 ±   0.2       5.2 ±   0.1
       Ash                  9.0 ±     0.1     8.0 ±   0.1     8.4 ±   0.004    8.2 ±   0.002       8.4 ±   0.001      8.6 ±   0.03     8.7 ±   0.1      8.9 ±   0.02     10.1 ±   0.1
       ANSb                35.7 ±     0.5    33.4 ±   0.6    32.9 ±   0.2     32.2 ±   0.2        33.8 ±   0.2       31.1 ±   0.5     33.3 ±   0.3     32.3 ±   0.1      31.7 ±   1.1
       AUAc                48.5 ±     1.2    53.1 ±   0.7    50.7 ±   0.7     55.2 ±   1.2        49.9 ±   0.8       54.9 ±   0.8     50.3 ±   1.0     58.0 ±   0.5      51.0 ±   1.2
       MeOHc               6.09 ±     0.23   7.27 ±   0.10   7.42 ±   0.11    7.30 ±   0.10       6.80 ±   0.10      7.16 ±   0.08    6.40 ±   0.24    6.74 ±   0.03     6.76 ±   0.08
       Acc                  0.55              0.71            0.78             0.72                0.76               0.67             0.69             0.50              0.63
Total (1) 105.4 107.3 105.2 108.9 105.1 107.9 104.7 112.0 105.4
       AUAtitr             38.2 ± 0.9        41.2 ± 0.2      40.2 ± 0.3       42.2 ± 0.6          37.5 ± 0.2         40.8 ± 0.1       40.5 ± 0.4       40.4 ± 0.9        38.9 ± 0.5
       MeOHtitr            4.69 ± 0.14       5.05 ± 0.03     4.93 ± 0.05      5.23 ± 0.10         4.68 ± 0.04        5.00 ± 0.02      5.06 ± 0.07      4.89 ± 0.16       4.82 ± 0.04
Total (2) 93.1 92.5 91.5 93.1 89.9 91.0 92.9 92.0 90.7
       ANS, total content of neutral sugars, calculated as their anhydro forms; AUAc, colorimetric anhydrogalacturonic acid content; MeOH, methoxyl content
       (as methanol); Ac, acetyl content (as acetic acid); AUAtitr, titrimetric anhydrogalacturonic acid content; MeOHtitr, titrimetric methylester content; Total
       (1), mass balance based on the contents of moisture, ash, ANS, AUAc, MeOH, and Ac; Total (2), mass balance based on the contents of moisture, ash,
       ANS, AUAtitr, and MeOHtitr.
       a
         Mean content ± standard error (SE) in g hg)1 of AIS (Ac: SE £ 0.01 g hg)1).
       b
         Including the glucose content of starch (cf. Table 1) and ribose (£ 0.24 g hg)1).
       c
        Quantified by HPLC.
       International Journal of Food Science and Technology 2010                                2010 The Authors. Journal compilation  2010 Institute of Food Science and Technology
                                                                                                                     Stability of mango peel by-products S. Sirisakulwat et al.             1653
                                      a
Table 3 Esterification indices of the alcohol-insoluble substance (AIS) extracted from dried peel waste (MPW) that accrued from the
industrial canning of ‘Kaew Khiew’ mango fruit after exposure of the wet peels to the ambient conditions of the peeling room (25 C, 63%
relative humidity) for different holding times (HT25 C) up to 5 h prior to waste stabilisation
Variant MPW1 MPW2 MPW3 MPW4 MPW5 MPW6 MPW7 MPW8 MPW9
DE (%)               69.7 ± 0.5           69.7 ± 0.1         69.6 ± 0.2         70.4 ± 0.4       70.8 ± 0.1            69.6 ± 0.1       71.0 ± 0.3        68.8 ± 0.7       70.4 ± 0.4
DMe (%)              69.0 ± 3.0           75.2 ± 1.4         80.5 ± 1.6         72.7 ± 1.9       74.9 ± 1.6            71.7 ± 1.3       69.9 ± 3.0        63.9 ± 0.7       72.8 ± 1.9
DAc (%)               3.3 ± 0.1            3.9 ± 0.1          4.5 ± 0.1          3.8 ± 0.1        4.5 ± 0.1             3.6 ± 0.1        4.1 ± 0.1         2.5 ± 0.02       3.6 ± 0.1
DE, degree of esterification (as molar MeOHtitr ⁄ AUAtitr ratio, cf. Table 2); DMe, degree of methylation (as molar MeOH ⁄ AUAc ratio, cf. Table 2); DAc,
degree of acetylation (as molar Ac ⁄ AUAc ratio, cf. Table 2).
a
  Mean ± standard error.
6.1–7.4 g hg)1) surpassed the titrimetric methylester                                            displaying a median of 72.7% (Table 3). Evidently, the
contents (MeOHtitr) by approximately 2 g hg)1                                                    two extreme DMe levels of 64% (MPW8) and 81%
(Table 2). As the respective mass balance averaged out                                           (MPW3) represented outliers ascribed to overestimated
at 106.8% [total (1), Table 2], especially the colorimetric                                      maximum contents of AUAc and MeOH, respectively,
anhydrogalacturonic acid contents were obviously over-                                           but were not causally related to the storage of the wet
estimated throughout this study, most notably in case of                                         peels at 25 C. Likewise, the DAc was unaffected by the
sample MPW8. Despite the deficiencies of the associated                                           storage of the wet peels, as shown by its slight variation
mass balance [total (2)] in this study, the precision of the                                     around a median of 3.8% (Table 3). In conformity with
titrimetric results (AUAtitr and MeOHtitr) of the nine                                           the nine AIS samples from industrial peel waste, the
samples overall appeared to be better than their AUAc                                            ‘Kaew Khiew’ peel pectin mentioned earlier for com-
and MeOH contents.                                                                               parison was characterised by a DE of 71.8 ± 0.1%, a
   Because the titrimetrically quantified DE of the                                               DMe of 77.8 ± 2.0%, and a DAc of 3.6 ± 0.1%
galacturonans closely varied around a median of                                                  (Sirisakulwat et al., 2008).
69.7% (Table 3), de-esterification by PME during peel                                               As detailed above, all nine AIS samples revealed
storage at 25 C was irrelevant. A DE of 70% was                                                 almost equal contents of anhydrogalacturonic acid and
uniformly observed when the wet peels had been dried                                             total neutral sugars (Table 2). Among the latter, galac-
without a dwell time at 25 C (MPW1) and after storage                                           tose (Gal) residues were by far prevailing (Table 4) with
for 5 h at this temperature (MPW9). Despite the                                                  a median of 145 mmol hg)1 of AISS-corr, corresponding
problems faced in this study with the colorimetric                                               to 23–25 g hg)1 of AISS-corr and 59–66 mol hmol)1 of
AUAc and the chromatographic MeOH analysis, the                                                  AUAtitr. Although the galactose contents seemed to
findings in terms of DE were confirmed by the DMe                                                  be maximum and minimum within that range after
                                a
Table 4 Molar sugar composition of the alcohol-insoluble substance on a starch-free basis (AISS-corr) after recovery from dried peel waste
(MPW) that accrued from the industrial canning of ‘Kaew Khiew’ mango fruit after exposure of the wet peels to the ambient conditions of the
peeling room (25 C, 63% relative humidity) for different holding times (HT25 C) up to 5 h prior to waste stabilisation
Variant MPW1 MPW2 MPW3 MPW4 MPW5 MPW6 MPW7 MPW8 MPW9
AUAc                292    ±   7           314    ±   7       299    ±   7      323   ±   9       296    ±   8         319   ±   9       296   ±   7      343   ±   11     301   ±   8
AUAtitr             230    ±   6           244    ±   4       237    ±   5      247   ±   5       223    ±   5         237   ±   6       238   ±   3      239   ±   9      230   ±   4
Gal                 151    ±   3           146    ±   5       145    ±   3      145   ±   3       142    ±   3         144   ±   5       145   ±   2      144   ±   5      139   ±   7
Ara                   16   ±   0             15   ±   0         17   ±   1       16   ±   0         21   ±   1          14   ±   0        19   ±   1       14   ±   0       17   ±   1
Glcb                  19   ±   2             15   ±   1         14   ±   1       14   ±   1         17   ±   1          12   ±   1        15   ±   1       15   ±   1       13   ±   2
Rha                  8.9   ±   0.1        10.6    ±   0.6    10.2    ±   0.3    9.9   ±   0.2      9.9   ±   0.2       9.8   ±   0.3    10.0   ±   0.3    9.0   ±   0.3    8.8   ±   0.7
Man                  1.8   ±   0.1          2.0   ±   0.04     2.1   ±   0.1    2.2   ±   0.1      2.4   ±   0.1       2.3   ±   0.1     2.2   ±   0.03   1.8   ±   0.1    1.9   ±   0.04
Xyl                  1.7   ±   0.03         2.0   ±   0.03     2.2   ±   0.04   1.8   ±   0.1      2.2   ±   0.1       2.0   ±   0.1     2.0   ±   0.1    1.5   ±   0.1    1.6   ±   0.03
Fuc                  0.4   ±   0.03         0.4   ±   0.01     0.4   ±   0.02   0.4   ±   0.01     0.5   ±   0.01      0.4   ±   0.01    0.5   ±   0.03   0.4   ±   0.01   0.4   ±   0.03
AUAc, galacturonic acid (colorimetric); AUAtitr, galacturonic acid (titrimetric); Gal, galactose; Ara, arabinose; Glc, glucose; Rha, rhamnose; Man,
mannose; Xyl, xylose; Fuc, fucose.
a
  Mean ± standard error in mmol hg)1 of AISS-corr.
b
  Without glucose included in starch.
 2010 The Authors. Journal compilation  2010 Institute of Food Science and Technology                             International Journal of Food Science and Technology 2010
1654   Stability of mango peel by-products S. Sirisakulwat et al.
       exposure of the wet peels to 25 C for 0 (MPW1) and                                  purification in acidic alcohol amounted to 56–59 g hg)1
       5 h (MPW9), respectively, constant levels were observed                              of AISp (Table 5), the nine samples did not meet the
       for the other seven AIS samples. On the whole, the nine                              JECFA minimum requirement as to the galacturonide
       pectins revealed, regardless of the storage of the wet peel                          content (65 g hg)1 of AISp; Joint FAO ⁄ WHO Expert
       waste, an almost identical neutral sugar composition                                 Committee on Food Additives (JECFA), 2007). How-
       (Table 4) as the peel pectin of the experimental ‘Kaew                               ever, the portions of homogalacturonans (HG) and rham-
       Khiew’ fruit batch cited earlier for comparison did                                  nogalacturonans (RG-I) were obviously not affected by
       (Sirisakulwat et al., 2008). Their arabinose (Ara) con-                              the wet peel storage, because largely constant molar
       tents slightly varied around a median of 16 mmol hg)1                                AUAtitr ⁄ Rha ratios of 23–26 occurred throughout, as
       of AISS-corr (i.e. 2.1 g hg)1), followed by median con-                              indicated by the respective sugar amounts displayed
       tents of 15, 9.9, 2.1, and 2.0 mmol hg)1 of AISS-corr                                in Table 4. Also the backbone indices (Table 5), which
       for glucose (Glc) not contained in starch, rhamnose                                  were estimated from the molar AUAc and rhamnose
       (Rha), mannose (Man), and xylose (Xyl), respectively                                 contents on the basis of a simplified backbone model
       (Table 4). Strongest variation among the nine samples                                consisting of HG and RG-I (Sirisakulwat et al., 2008),
       was observed for arabinose and the nonstarch glucose                                 did not point to any significant backbone degradation
       contents. However, no impact of wet peel storage was                                 due to the wet peel storage, because largely constant
       noticed.                                                                             maximum percentages of the pectin backbone resulted
         As shown previously (Neidhart et al., 2009), galactose                             for homogalactacuronans (BBPHG, 93.4–94.9%) and
       contents of mango peel pectins may be considerably high,                             rhamnogalacturonans type I (BBPRG-I, 5.1–6.6%). If all
       but they seemed to be specific to the cultivar and were                               galactose residues were ascribed to galactans with one
       neither affected by fruit ripeness nor by the extraction                              chain branching off from each rhamnose unit of rham-
       mode. Thus, even in the presence of minor natural starch                             nogalacturonans type I, long and ⁄ or highly ramified
       contents, the galacturonide content of mango peel AIS                                galactan side chains of 14–17 residues may be assumed
       may markedly be limited. This feature also applied to the                            according to the molar Gal ⁄ Rha ratios (Table 5). This
       nine AIS samples of this study. Because their galact-                                striking peculiarity and the AUAtitr ⁄ Rha ratio, observed
       uronic acid contents (GalUAtitr, Mr = 194.1 g mol)1)                                 here for AIS from industrial peel waste, confirmed
       on an ash- and moisture-free base (AISp) after pectin                                the former report (Sirisakulwat et al., 2008) for the
                                 a
       Table 5 Structural indices of the alcohol-insoluble substance (AIS) extracted from dried peel waste (MPW) that accrued from the industrial
       canning of ‘Kaew Khiew’ mango fruit after exposure of the wet peels to the ambient conditions of the peeling room (25 C, 63 % relative humidity)
       for different holding times (HT25 C) up to 5 h prior to waste stabilisation
Variant MPW1 MPW2 MPW3 MPW4 MPW5 MPW6 MPW7 MPW8 MPW9
                           )1
       GalUAtitr (g hg of AISp)    55.5 ±    1.3     58.2 ± 0.3    56.7 ± 0.4     59.0 ± 0.8     58.5 ± 0.3       58.5 ± 0.2       59.2 ± 0.6     58.8 ± 1.4       58.1 ± 0.8
       Molecular parameters
          [g] (mL g)1)              282 ±    2        317 ± 2       341 ± 2       329 ± 2         334 ± 2          308 ± 2          325 ± 3        276 ± 2          271 ± 2
       Side chain indices
         Ara ⁄ Rha (mol mol)1)       1.8 ±   0.02     1.4 ± 0.1     1.7 ± 0.1      1.6 ± 0.04     2.1 ± 0.04       1.5 ± 0.03       1.9 ± 0.1      1.5 ± 0.03       1.9 ± 0.2
         Gal ⁄ Rha (mol mol)1)     16.9 ±    0.3     13.8 ± 0.8    14.2 ± 0.4     14.6 ± 0.1     14.2 ± 0.1       14.7 ± 0.4       14.5 ± 0.4     16.0 ± 0.3       15.7 ± 1.4
         Ara ⁄ Gal (mol hmol)1)    10.7 ±    0.2     10.4 ± 0.3    11.7 ± 0.5     11.1 ± 0.3     14.4 ± 0.3       10.0 ± 0.3       12.9 ± 0.3      9.5 ± 0.1       12.2 ± 0.7
       Backbone indices (of AISS-corr)
         HGmaxb (mmol hg)1)         283 ±    7        304 ± 7       288 ± 7        313 ± 9        286 ± 8          309 ± 9         286 ± 7         334 ± 11        293 ± 8
         RG-Imaxc (mmol hg)1)      17.9 ±    0.2     21.1 ± 1.1    20.4 ± 0.7     19.8 ± 0.3     19.9 ± 0.4       19.6 ± 0.5       20.1 ± 0.5     17.9 ± 0.7       17.6 ± 1.3
         BBPHGd (%)                  94.1             93.5          93.4           94.1           93.5             94.0             93.4           94.9             94.3
         BBPRG-Ie (%)                  5.9             6.5           6.6            5.9            6.5              6.0              6.6            5.1              5.7
       GalUAtitr, titrimetric galacturonic acid content (g hg)1 of AISp, i.e., of nondestarched AIS after acidic purification before titration); [g], intrinsic viscosity
       (AIS dissolved in 0.28 M KOAc ⁄ HOLc buffer, pH 3.0); Ara, arabinose (mmol hg)1 of AIS); Rha, rhamnose (mmol hg)1 of AIS); Gal, galactose (mmol hg)1
       of AIS).
       a
         Mean ± standard error.
       b
         Estimated maximum units of the total homogalacturonan backbone (HG) calculated from the AUAc and Rha contents in mmol hg)1 of AISS-corr
       (HGmax = AUAc-Rha).
       c
        Estimated maximum units of the total rhamnogalacturonan-I backbone (RG-I) calculated from the Rha content in mmol hg)1 of AISS-corr
       (RG-Imax = 2 Rha).
       d
         Maximum homogalacturonan (HG) percentage of the pectin backbone [BBPHG = 100(AUAc ) Rha)/(AUAc + Rha)].
       e
         Maximum rhamnogalacturonan-I (RG-I) percentage of the pectin backbone [BBPRG)I = 100(2ÆRha)/(AUAc + Rha)].
       International Journal of Food Science and Technology 2010                         2010 The Authors. Journal compilation  2010 Institute of Food Science and Technology
                                                                                                     Stability of mango peel by-products S. Sirisakulwat et al.   1655
analogously extracted peel AIS from the experimental                                      Table 5 clearly exceeded the intrinsic viscosity of the
‘Kaew Khiew’ fruit batch. But galactan degradation                                        reported ‘Kaew Khiew’ peel pectin (234 mL g)1), which
during storage of the wet peels by b-d-galactosidase                                      had displayed a large arabinogalactan fraction [(Ara +
activities was obviously negligible under the conditions                                  Gal) ⁄ Rha = 19.2] similar to the MPW1 pectin, but only
applied. Because of the acid-lability of arabinofuranosyl                                 molar AUA ⁄ Rha ratios of 23 and 24 based on AUAc
linkages, arabinose residues are more or less split off                                    and AUAtitr, respectively (Sirisakulwat et al., 2008). As
during hot-acid extraction, depending on the pH condi-                                    previously shown for this pectin by high-performance
tions applied (Sirisakulwat et al., 2008; Neidhart et al.,                                size exclusion chromatography, its comparatively low
2009). However, like the Gal ⁄ Rha ratios, also molar                                     intrinsic viscosity resulted from the co-existence of two
Ara ⁄ Rha ratios of 1.4–2.1 around a median of 1.7 mol ⁄ -                                distinct major fractions. Apart from a high-molecular
mol and Ara ⁄ Gal ratios of 10–14 mol hmol)1 (Table 5)                                    weight fraction also found in commercial apple pectin,
pointed to insignificant side-chain degradation during the                                 an additional, almost monodisperse fraction with a peak
storage of the wet peels.                                                                 molecular weight of 17 000 relative to dextran consid-
   The clearest evidence for the preservation of pectin                                   erably reduced the average molecular weight of this
backbones and side chains during the storage of the wet                                   pectin (Sirisakulwat et al., 2008). Depending on the
peels at 25 C was finally provided by the intrinsic                                       amounts of this characteristic fraction, the gelling and
viscosities ([g]) of the samples (Table 5). Within a range                                thickening properties of mango peel pectins may be
of 271–341 mL g)1, [g] closely varied around a median                                     more or less limited, as demonstrated by numerous
of 317 mL g)1, indicating good consistency among the                                      samples (Neidhart et al., 2009).
nine pectins in terms of their average molecular dimen-
sions (Morris, 1995). The lowest intrinsic viscosities
                                                                                          Impact of peel storage on techno-functional pectin
(271–282 mL g)1) were observed for the AIS group
                                                                                          properties
from the three peel waste samples collected within the
first 64 min of sampling (MPW1, MPW8, MPW9,                                                From the similarities in the average composition
Fig. 1), including the extreme situations, i.e. immediate                                 (Tables 2-4) and the intrinsic viscosity reflecting the mean
stabilisation and exposure to 25 C for 5 h prior to                                      molecular weight (Table 5), no differences in the techno-
drying, respectively. Thus, the slight differences among                                   functional properties were expected among the nine
the nine pectins were definitely ascribed to the inherent                                  pectins. On the other hand, weak activities of the
heterogeneity of the fruits and the reproducibility of                                    respective esterases and depolymerising hydrolyses and
pectin recovery (Sirisakulwat et al., 2008) rather than to                                lyases may nevertheless cause enhanced variation among
the storage of the wet peels at ambient temperature. The                                  the molecules in terms of molecular size, side-chain
rhamnose contents were slightly lower in the AIS from                                     lengths, and the degrees of methylation and acetylation.
the peel samples MPW1, MPW8, and MPW9 (approx-                                            Likewise, the intramolecular distribution of methyl-
imately 9 mmol hg)1 of AISS-corr, Table 4) compared to                                    esterified units might be affected, especially because of
the remaining pectins. Owing to the minor variation of                                    the blockwise mode of action of plant PME (Benen et al.,
galactose contents, these three pectins were further                                      2003a). Owing to such differences in their fine structure
characterised by maximum Gal ⁄ Rha ratios (Fig. 1).                                       (Guillotin et al., 2007), pectins with similar average
Thus, their arabinogalactan side chains were possibly                                     characteristics may display different gelling behaviour
more extended than in the other cases, as equally                                         (Neidhart et al., 2003).
indicated by their molar (Ara+Gal) ⁄ Rha ratios of                                          Consistent with their low galacturonide contents
18–19 relative to 15–16 for the other pectins (Table 5).                                  (Table 2) and intrinsic viscosities (Table 5), the nine
The intrinsic viscosity would consistently decline along                                  samples produced only soft gels. Low breaking strengths
with a relative increase in branched neutral sugar side                                   of 369–497 HPE resulted even at an AIS dose of
chains due to overall more condensed coil dimensions                                      0.3 g hg)1 of gel (BS0.3%; Table 6) and 0.35 g hg)1 were
(Morris, 1995). In the present case, this seemed to be                                    necessary to achieve BSs of 452–594 HPE (BS0.35%). As
partly compensated by more expanded homogalacturo-                                        displayed by the AIS amounts required for 100 g of a
nan parts, because especially the AIS from MPW8 and                                       standard gel with a BS of 530 HPE, the nine samples
MPW9 besides MPW1 also displayed elevated molar                                           were quite uniform in terms of their breaking capacities
AUA ⁄ Rha ratios (both on the basis of the AUAtitr and                                    (BC530HPE; Table 6). With a BC530HPE range of 0.33–
the AUAc contents; Fig. 1). Nevertheless, their lower                                     0.4 g hg)1 of gel, the breaking capacity of the ‘Kaew
intrinsic viscosities were most probably owing to larger                                  Khiew’ peel AIS reported as a reference was confirmed;
arabinogalactan parts, because the MPW1 AIS came                                          but compared to a commercial, unstandardised apple
quite close to the MPW4 and MPW6 samples in terms                                         pectin that was also included in the previous study
of the AUA ⁄ Rha ratios despite the significantly higher                                   (Sirisakulwat et al., 2008), 1.9–2.4 times more AIS was
intrinsic viscosities of the latter group ([g] ‡ 308 mL g)1;                              needed to produce this standard gel. Consequently, the
Fig. 1). Both the maximum and minimum [g] levels in                                       sugar amount bound in a sugar-acid standard gel by 1 g
 2010 The Authors. Journal compilation  2010 Institute of Food Science and Technology             International Journal of Food Science and Technology 2010
1656   Stability of mango peel by-products S. Sirisakulwat et al.
       Table 6 Gelling capacity of the alcohol-insoluble substance (AIS) extracted from dried peel waste (MPW) that accrued from the industrial
       canning of ‘Kaew Khiew’ mango fruit after exposure of the wet peels to the ambient conditions of the peeling room (25 C, 63 % relative
       humidity) for different holding times (HT25 C) up to 5 h prior to waste stabilisation
Variant MPW1 MPW2 MPW3 MPW4 MPW5 MPW6 MPW7 MPW8 MPW9
       Gelling capacity of the AIS and the dried raw material (DRM), respectively
        BS0.3% (HPE)                            458 ± 3a      478 ± 2      369 ± 3      399 ± 5     463 ± 9                        497 ± 8     463 ± 6      416 ± 4        394 ± 1
        BS0.35% (HPE)                           586 ± 5a      564 ± 13     452 ± 8      594 ± 5     570 ± 6                        563 ± 4     587 ± 14     528 ± 6        509 ± 2
        BC530HPE (g hg)1)                       0.33          0.33         0.40         0.33        0.33                           0.33        0.33         0.35           0.36
        SBC530HPE (g g)1 of AIS)                198           197          164          195         196                            200         199          185            181
        SBCDRM (g hg)1)                         2951          3062         2644         3066        3092                           3108        3124         2717           2935
       Normalised gelling capacity of the AIS relative to the AUAtitr content of the standardised gel with 530                    HPE
        BC530HPE(AUAtitr) (g hg)1)              0.13          0.14         0.16         0.14        0.12                           0.13        0.13         0.14           0.14
        SBC530HPE(AUAtitr) (g g)1 of AUA)       519           478          407          462         523                            490         491          459            465
       a
         Mean ± standard error. BS0.3% and BS0.35%, breaking strength of gels with AIS doses of 0.3 and 0.35% (w ⁄ w), respectively, in Herbstreith-Pectinometer
       units (HPE); BC530HPE, breaking capacity of the AIS as gram of AIS required for 100 g of a gel with 530 HPE; SBC530HPE, sugar-binding capacity of
       the AIS as gram of sugar bound per gram of AIS in a gel of 530 HPE; SBCDRM, gelling units (GU) of the dried raw material (DRM; here: MPW) as its
       sugar-binding capacity in gram of sugar bound by 100 g of DRM in a gel of 530 HPE; BC530HPE(AUAtitr), normalised breaking capacity of the AIS
       (g of AUA hg)1 of a gel with 530 HPE); SBC530HPE(AUAtitr), normalised sugar-binding capacity of the AIS (g of sugar g)1 of AUA for a gel of 530 HPE).
       of this apple pectin exceeded the sugar-binding capacities                     ison to pectins with improved techno-functionality from
       (SBC530HPE) of the nine mango AIS samples (164–                                other mango peels (Neidhart et al., 2009).
       200 g g)1; Table 6) by the same factors. Because of their                         Like the gel properties, the setting behaviour of the
       uniform AIS yields (AISS-corr; Table 1) that slightly                          AIS was also not verifiably affected by the intermediate
       exceeded that of this former ‘Kaew Khiew’ peel sample                          exposure of the wet peels to ambient temperature.
       (13.1 ± 0.2 g hg)1; Sirisakulwat et al., 2008), the dried                      Despite some variation of the setting temperature that
       peels MPW1-MPW9 had the capacity to bind more sugar                            was more pronounced at the upper AIS dose, equally
       in a standard gel by the recovered AIS than the latter                         high setting temperatures were recorded for AIS that
       (SBCDRM; 2644–3124 vs. 2250 g hg)1 of dried peel;                              was obtained from peels after their wet storage at 25 C
       Table 6). Thus, the industrial peel waste yielded slightly                     for 0, 15, and 300 min (Fig. 2).
       more AIS than the cited peel sample, but of comparable
       quality. The three samples displaying minimum intrin-
       sic viscosities of the extractable AIS (MPW1, MPW8,                                                        45
       MPW9; Fig. 1) were among the four samples with a                                                           40
       SBCDRM below the median. However, together with the
                                                                                         T (δ1.0 Hz = 45°) (°C)
                                                                                                                  35
       other AIS samples from industrial peel waste, their AIS
                                                                                                                  30
       was almost identical to that of the cited ‘Kaew Khiew’
       peel sample (0.14 g hg)1; Sirisakulwat et al., 2008) and                                                   25
       International Journal of Food Science and Technology 2010                     2010 The Authors. Journal compilation  2010 Institute of Food Science and Technology
                                                                                                       Stability of mango peel by-products S. Sirisakulwat et al.    1657
Conclusion                                                                                Acknowledgments
The findings reported for mango peel AIS from exper-                                       This research was funded by Deutsche Forschungs-
imental fruit batches (Sirisakulwat et al., 2008; Neidhart                                gemeinschaft, Bonn, Germany: Project SFB 564-E2.2. It
et al., 2009) were overall confirmed by industrial                                         is part of the Special Research Program ‘Research for
by-products from the fruit of a further crop year. Most                                   Sustainable Land Use and Rural Development in
important, temporary exposure of wet mango peels to                                       Mountainous Regions of Southeast Asia’ (The Uplands
ambient temperature was innocuous in terms of yield,                                      Program).
composition, and techno-functionality of the extract-                                        The authors thank Herbstreith & Fox KG, Neu-
able AIS. The interim storage of the wet peel waste in                                    enbürg, Germany, in particular Hans-Ulrich Endress
the peeling room prior to drying can thus be tolerated                                    and Christine Rentschler, for providing laboratory
even up to 5 h without notable pectin degradation.                                        facilities for pectin extraction as well as Northern Food
Limited tissue damage during manual peeling and low                                       Co., Ltd., Chiang Mai, Thailand for supplying MPW.
activities of degrading endogenous enzymes in the peels                                   Klaus Mix and Martin Leitenberger are acknowledged
(Yanru et al., 1995) might support this storage stability.                                for their technical assistance with the experiments at
On a relatively large part of the peel waste surface, wax                                 Hohenheim University.
layers and the thickness of the cuticle initially still act as
physical barriers. Additionally, minor antimicrobial
                                                                                          References
effects might still emanate from polyphenolics like
gallotannins and alk(en)ylresorcinols present in mango                                    Ali, Z.M., Chin, L.-H. & Lazan, H. (2004). A comparative study on
peels even at consumption ripeness of the fruit (Berar-                                     wall degrading enzymes, pectin modifications and softening during
                                                                                            ripening of selected tropical fruits. Plant Science, 167, 317–327.
dini et al., 2004; Engels et al., 2009; Knödler et al.,                                  Benen, J.A.E., van Alebeek, G.-J.W.M., Voragen, A.G.J. & Visser, J.
2009). Compared to twelve other mango cultivars, peels                                      (2003a). Pectic esterases. In: Handbook of Food Enzymology (edited
of ‘Kaew’ fruit were reported to be comparatively rich                                      by J.R. Whitaker, A.G.J. Voragen & D.W.S. Wong). Pp. 849–856.
in alk(en)ylresorcinols (1.4 g kg)1 of peel dry matter;                                     New York, NY, USA: Marcel Dekker.
                                                                                          Benen, J.A.E., Voragen, A.G.J. & Visser, J.. (2003b). Pectic enzymes.
Knödler et al., 2009), which play a role in plant disease                                  In: Handbook of Food Enzymology (edited by J.R. Whitaker, A.G.J.
resistance (Hassan et al., 2007). Because of the en-                                        Voragen & D.W.S. Wong). Pp. 845–848. New York, NY, USA:
hanced flexibility, the observed tolerance of intermedi-                                     Marcel Dekker.
ate storage is important for a future exploitation of peel                                Berardini, N., Carle, R. & Schieber, A. (2004). Characterization of
waste from mango processing on smaller industrial                                           gallotannins and benzophenone derivatives from mango (Mangifera
                                                                                            indica L. cv. ‘Tommy Atkins’) peels, pulp and kernels by high-
scales, where immediate peel drying may impose con-                                         performance liquid chromatography ⁄ electrospray ionization mass
siderably higher logistic and economic investment than                                      spectrometry. Rapid Communications in Mass Spectrometry, 18,
on large scale with completely continuous processing                                        2208–2216.
and waste stabilisation. As mango residues result from                                    Berardini, N., Fezer, R., Conrad, J., Beifuss, U., Carle, R. & Schieber,
                                                                                            A. (2005a). Screening of mango (Mangifera indica L.) cultivars for
multifaceted processing on different scales, the precon-                                     their contents of flavonol O- and xanthone C-glycosides, anthocya-
ditions for economic by-product drying are rather                                           nins, and pectin. Journal of Agricultural and Food Chemistry, 53,
individual. Knowledge about the susceptibility of indus-                                    1563–1570.
trial mango peels to pectin degradation prior to drying                                   Berardini, N., Knödler, M., Schieber, A. & Carle, R. (2005b).
is of utmost importance for the selection of adjusted                                       Utilization of mango peels as a source of pectin and polyphenolics.
                                                                                            Innovative Food Science and Emerging Technologies, 6, 442–452.
drying technologies and economic concepts for the                                         Brummell, D.A. (2006). Cell wall disassembly in ripening fruit.
overall processes.                                                                          Functional Plant Biology, 33, 103–119.
   The interim storage of the wet mango peels neither                                     Chourasia, A., Sane, V.A. & Nath, P. (2006). Differential expression of
caused perceptible variations in pectin quality nor the                                     pectate lyase during ethylene-induced postharvest softening of
                                                                                            mango (Mangifera indica var. Dashehari). Physiologia Plantarum,
comparably inferior galacturonide contents and gelling                                      128, 546–555.
capacities of the pectins, which were observed in spite of                                De Vries, R.P. & Visser, J. (2003). Enzymes releasing L-arabinose and
hot-acid extraction that mimicked industrial procedures                                     D-galactose from the side chains of pectin. In: Handbook of Food
for pectin recovery from established sources. Despite                                       Enzymology (edited by J.R. Whitaker, A.G.J. Voragen & D.W.S.
individual promising findings based on laboratory                                            Wong). Pp. 867–877. New York, NY, USA: Marcel Dekker.
                                                                                          Endress, H.-U. & Dilger, S. (1990). Checking pectin jelly strength with
extraction (Rehman et al., 2004; Koubala et al., 2009;                                      the Pektinometer. Food Technology International, 1, 279–282.
Neidhart et al., 2009), quality deficiencies of mango peel                                 Endress, H.-U., Mattes, F. & Norz, K. (2006). Pectins. In: Handbook
pectin, which have repeatedly been reported (Pedroza-                                       of Food Science, Technology, and Engineering (edited by Y.H. Hui),
Islas et al., 1994) as in the present case, require further                                 Vol. 3. Pp. 140 ⁄ 1–140 ⁄ 35. Boca Raton, FL, USA: CRC Press,
                                                                                            Taylor & Francis Group.
studies. Research into sustainable recovery of purified                                    Engels, C., Knödler, M., Zhao, Y.-Y., Carle, R., Gänzle, M.G. &
pectins from mango peels like those used in the present                                     Schieber, A. (2009). Antimicrobial activity of gallotannins isolated
and previous trials (Sirisakulwat et al., 2008) are                                         from mango (Mangifera indica L.) kernels. Journal of Agricultural
currently under way.                                                                        and Food Chemistry, 57, 7712–7718.
 2010 The Authors. Journal compilation  2010 Institute of Food Science and Technology               International Journal of Food Science and Technology 2010
1658   Stability of mango peel by-products S. Sirisakulwat et al.
       Guillotin, S.E., Bakx, E.J., Boulenguer, P., Schols, H.A. & Voragen,        Panouillé, M., Ralet, M.-C., Bonnin, E. & Thibault, J.-F. (2007).
         A.G.J. (2007). Determination of the degree of substitution, degree of       Recovery and reuse of trimmings and pulps from fruit and vegetable
         amidation and degree of blockiness of commercial pectins by using           processing. In: Handbook of Waste Management and Co-product
         capillary electrophoresis. Food Hydrocolloids, 21(3), 444–451.              Recovery in Food Processing (edited by K. Waldron), Vol. 1. Pp.
       Hassan, M.K., Dann, E.K., Irving, D.E. & Coates, L.M. (2007).                 417–447. Cambridge, UK: Woodhead.
         Concentrations of constitutive alk(en)ylresorcinols in peel of com-       Pedroza-Islas, R., Aquilar-Esperanza, E. & Vernon-Carter, E.J.
         mercial mango varieties and resistance to postharvest anthracnose.          (1994). Obtaining pectins from solids wastes derived from mango
         Physiological and Molecular Plant Pathology, 71, 158–165.                   (Mangifera indica) processing. AIChE Symposium Series, 300, 36–41.
       Joint FAO ⁄ WHO Expert Committee on Food Additives (JECFA)                  Pott, I., Neidhart, S., Mühlbauer, W. & Carle, R. (2005). Quality
         (2007). Compendium of Food Additive Specifications. FAO JECFA                improvement of non-sulphited mango slices by drying at high
         Monographs 4. Rome, Italy: Food and Agriculture Organization                temperatures. Innovative Food Science & Emerging Technologies,
         of the United Nations. http://www.fao.org/docrep/010/a1447e/                6(4), 412–419.
         a1447e00.htm.                                                             Prasanna, V., Prabha, T.N. & Tharanathan, R.N. (2006). Multiple
       Knödler, M., Reisenhauer, K., Schieber, A. & Carle, R. (2009).               forms of polygalacturonase from mango (Mangifera indica L. cv.
         Quantitative determination of allergenic 5-alk(en)yl-resorcinols in         Alphonso) fruit. Food Chemistry, 95, 30–36.
         mango (Mangifera indica L.) peel, pulp, and fruit products by high-       Rehman, Z.U., Salariya, A.M., Habib, F. & Shah, W.H. (2004).
         performance liquid chromatography. Journal of Agricultural and              Utilization of mango peels as a source of pectin. Journal of the
         Food Chemistry, 57, 3639–3644.                                              Chemical Society of Pakistan, 26(1), 73–76.
       Koubala, B.B., Kansci, G., Mbome, L.I., Crépeau, M.-J., Thibault,          Singh, P. & Dwivedi, U.N. (2008). Purification and characterization of
         J.-F. & Ralet, M.-C. (2008). Effect of extraction conditions on some         multiple forms of polygalacturonase from mango (Mangifera indica
         physicochemical characteristics of pectins from ‘‘Améliorée’’ and         cv. Dashehari) fruit. Food Chemistry, 111, 345–349.
         ‘‘Mango’’ mango peels. Food Hydrocolloids, 22(7), 1345–1351.              Sirisakulwat, S., Nagel, A., Sruamsiri, P., Carle, R. & Neidhart, S.
       Koubala, B.B., Kansci, G., Garnier, C., Mbome, I.L., Durand, S.,              (2008). Yield and quality of pectins extractable from the peels of
         Thibault, J.-F. & Ralet, M.-C. (2009). Rheological and high gelling         Thai mango cultivars depending on fruit ripeness. Journal of
         properties of mango (Mangifera indica) and ambarella (Spondias              Agricultural and Food Chemistry, 56(22), 10727–10738.
         cythera) peel pectins. International Journal of Food Science and          Sudhakar, D.V. & Maini, S.B. (2000). Isolation and characterization
         Technology, 44, 1809–1817.                                                  of mango peel pectins. Journal of Food Processing and Preservation,
       Kratchanova, M., Bénémou, C. & Kratchanov, C. (1991). On the                24(3), 209–227.
         pectic substances of mango fruits. Carbohydrate Polymers, 15,             Vásquez-Caicedo, A.L., Neidhart, S. & Carle, R. (2004). Postharvest
         271–282.                                                                    ripening behavior of nine Thai mango cultivars and their
       MacDougall, A.J. & Ring, S.G. (2004). Pectic polysaccharides. In:             suitability for industrial applications. Acta Horticulturae, 645,
         Chemical and Functional Properties of Food Saccharides (edited by           617–625.
         P. Tomasik). Pp. 181–195. Boca Raton, FL, USA: CRC Press.                 Vásquez-Caicedo, A.L., Heller, A., Neidhart, S. & Carle, R. (2006).
       Morris, E.R. (1995). Polysaccharide rheology and in-mouth percep-             Chromoplast morphology and b-carotene accumulation during
         tion. In: Food Polysaccharides and Their Applications (edited by            postharvest ripening of mango cv. ‘Tommy Atkins’. Journal of
         A.M. Stephen). Pp. 517–546. New York, NY, USA: Marcel Dekker.               Agricultural and Food Chemistry, 54, 5769–5776.
       Neidhart, S., Hannak, C. & Gierschner, K. (2003). Sol-gel transition        Vásquez-Caicedo, A.L., Schilling, S., Carle, R. & Neidhart, S. (2007).
         of high-esterified pectins and their molecular structure. In: Advances       Effects of thermal processing and fruit matrix on b-carotene stability
         in Pectin and Pectinase Research (edited by A.G.J. Voragen, H.A.            and enzyme inactivation during transformation of mangoes into
         Schols & R. Visser). Pp. 431–448. Dordrecht, The Netherlands:               purée and nectar. Food Chemistry, 102(4), 1172–1186.
         Kluwer Academic Publishers.                                               Voragen, A.G.J., Pilnik, W., Thibault, J.-F., Axelos, M.A.V. &
       Neidhart, S., Sirisakulwat, S., Nagel, A., Sruamsiri, S. & Carle, R.          Renard, C.M.G.C.. (1995). Pectins. In: Food Polysaccharides and
         (2009). Which mango processing residues are suitable for pectin             Their Applications (edited by A.M. Stephen). Pp. 287–339. New
         recovery in terms of yield, molecular and techno-functional                 York, NY, USA: Marcel Dekker.
         properties of extractable pectins? In: Pectins and Pectinases             Yanru, Z., Pandey, M., Prasad, N.K. & Srivastava, G.C. (1995).
         (edited by H.A. Schols, R.G.F. Visser & A.G.J. Voragen). Pp.                Ripening associated changes in enzymes and respiratory activities in
         177–195. Wageningen, The Netherlands: Wageningen Academic                   three varieties of mango (Mangifera indica L.). Indian Journal of
         Publishers.                                                                 Plant Physiology, 38(1), 73–76.
International Journal of Food Science and Technology 2010 2010 The Authors. Journal compilation 2010 Institute of Food Science and Technology