ERUDITIO Vol. 4, No.

2, Juni 2024
P-ISSN: 2580-7722 | E-ISSN: 2807-6222

analytical method No. 12/KO/10 on the Identification of 1,4-Dioxane in cosmetic products

by Gas Chromatography-Mass Spectroscopy was developed. Then it followed the updated
one on No. 44/KO/MA-PPPOMN/18 with a shifted purpose, from identification to
determination of levels in anticipation of changes in the regulation of 1,4-Dioxane as a
contaminant that has a maximum limit, then refined by adding internal standard (IS)
Tetrahydrofuran written in AM number 22/KO/MA-PPPOMN/20. Finally, this analytical
method has been refined again by replacing the IS using the isotope of 1,4-Dioxane, 1,4-
Dioxane-d8, with AM No. 01 /KO/MA-PPPOMN/22. This IS replacement regarded to
feedback from several ASEAN members to create the ASEAN Cosmetic Method (ACM).
The comparison between the applicable regulations and the developed AM as illustrated in
Table 5.
3.6 Regional Harmonization of 1,4-Dioxane Methods
To strengthen the testing capabilities of 1,4-Dioxane, stakeholders need an
analytical method that can be used for both pre and post-market surveillance. Indonesia, in
this case, CNQLDF, was appointed as the leader in the development of 1,4-Dioxane AM
for ASEAN (ASEAN Cosmetic Method, ACM). The process of establishing this ACM has
gone through a long process, according to the ASEAN Guideline on Establishing the
ASEAN Cosmetic Method (ACM). The establishment of ACM is carried out through
several stages of activities, starting from identifying ASEAN member states (AMS) with
related MAs, then comparing these AMs, and selecting the best AM, including the
validation results. Indonesian AM have the best sensitivity, thus it was chosen due to Gas
Chromatography Tandem Mass Spectrometry-Head Space (GCMS-HSS) has been selected
as the preferred instrument to become ACM candidates. The next step was to refine the
MA, in this case, making internal changes to the standards used, according to input from
other AMS in the ACTLC meeting. AM revalidation was then carried out using the internal
standard isotope of 1,4-Dioxane 1,4-Dioxane-d8. After the AM revalidation stage was
carried out, the collaboration test of the AM was continued. Furthermore, a manuscript
report was made along with a draft ACM. Input was sought from other AMS on the report
manuscript and draft ACM, which were then finalized by adopting the AM into ACM.
The collaborative study conducted from August to September 2022. It was attended by 10
participants, consisting of three ASEAN member countries, namely the Philippines,
Thailand, and Viet Nam, and seven laboratories in Indonesia, namely Indonesian FDA
provincial offices in Padang, DKI Jakarta, Pontianak, Denpasar, Mataram, Pangkal Pinang
and CNQLDF. The test objects were taken from products on the market and met the
homogeneity and stability test requirements. The collaboration test results are sr=0.14393;
sR=1.74388; RSDR=14.5010; PRSD=11.00388; HORRAT=1.318, or it can be concluded

AM validation results for determining 1,4-Dioxane levels in cosmetic products using

GCMS-HSS gave the following values (Table 6).

98 Susan Gracia Arpan, Sri Purwaningsih, Hasti Kusuma,

Erita Lusianti, Yustina Yustina
Strengthening the Surveillance of 1,4-Dioxane Contaminants in Cosmetics through Harmonization of
Analysis Methods and Networking of Cosmetics Laboratories in Indonesia
 ERUDITIO Vol. 4, No. 2, Juni 2024
P-ISSN: 2580-7722 | E-ISSN: 2807-6222

Table 6. 1,4-Dioxane Validation Parameter Value

Validation
No. Acceptance Condition GCMS Study
Parameters
1 Selectivity Resolution Rt 1,4- Dioxane 8.816, Rt 1,4- Dioxane -d8
8.704
m/z 1,4-Dioksan 88, 58, 43

m/z 1,4- Dioxane -d8 96, 64, 46

2 Linearity r = 1.000; Vx0 = 1.4%

3 Precision 0,3%

1,1%

0,2%

4 Accuracy – 110 94,6 – 95,7

-110 99,4 – 101,0

-110 101,7 – 102,1

5 LOD - 0,

6 LOQ - 0,

3.7 Harmonization of 1,4-Dioxane Method at the National Level

Through the notification system, the industry is fully responsible for the quality,
safety, and benefits of the products produced. One of the efforts to strengthen pre-market
supervision is to build cross-sectoral cooperation to strengthen industrial laboratories and
external laboratories that carry out cosmetic testing.
To date, 15 external laboratories have their cosmetic testing performance accredited
ISO 17025: 2017. Of these 15 laboratories, only two laboratories could carry out 1,4-
Dioxane testing. Therefore, it is necessary to strengthen pre-market supervision by
conducting cross-sector collaboration within the ICLN to equalize the ability of cosmetic
testing among laboratories. Some of the collaboration steps taken were as follows:
a. Training on validation of analytical methods to equalize perception in carrying out AM
validation
b. Technical training on cosmetic testing to improve personnel competency in conducting
cosmetic testing or implementing new AM.
c. Implementation of proficiency test to assess laboratory performance
d. Organization of collaboration tests to assess the robustness of analytical methods
e. Development of the ICLN website as a forum for all members to exchange information
about cosmetic testing
f. Harmonization of AM, both at the national, ASEAN regional, and international levels
Harmonization of analytical methods at the national, regional, and international
levels is an effort to harmonize existing analytical methods so that all laboratories have the
same reference standard for analytical methods when conducting sample testing. The
objectives of standardization according to RI Law No. 20/2014 were as follows:

Susan Gracia Arpan, Sri Purwaningsih, Hasti Kusuma, 99

Erita Lusianti, Yustina Yustina
Strengthening the Surveillance of 1,4-Dioxane Contaminants in Cosmetics through Harmonization of
Analysis Methods and Networking of Cosmetics Laboratories in Indonesia
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a. Improve quality assurance, production efficiency, national competitiveness, fair and

transparent business competition in trade, business certainty, and the ability of business
actors, as well as the ability of technological innovation.
b. Increasing protection to consumers, business actors, labor, and other communities, as
well as the state, both from the aspects of safety, security, health, and preservation of
environmental functions
c. Increase certainty, smoothness, and efficiency of trade transactions in goods and
services domestically and abroad
Harmonization of cosmetic analysis methods at the national level is carried out
through the issuance of Indonesian National Standards (INS). INS on Cosmetics can
prevent disputes over test results and increase the competitiveness of the nation's products.
The formulation of analytical methods into INS involves various stakeholders who are
members of the Cosmetics Technical Committee, consisting of representatives from
NQCLDF, Directorate of Standardization and Quality Control - Ministry of Trade, Center
for Standardization and Services for the Chemical, Pharmaceutical and Packaging
Industries - Ministry of Industry, Academic Experts from the University of Indonesia, PT
Saraswati Indo Genetech, PT SGS Indonesia, PT Angler BioChemlab, Indonesian
Cosmetics Association (Perkosmi), Indonesian Consumers Foundation (ICF).
To increase the capacity of 1,4-Dioxane testing in Indonesia, the Indonesian FDA
needs to harmonize the analytical testing methods for 1,4-Dioxane contamination at the
national level by issuing the Indonesian National Standards (INS). This ACM method is
intended to be widely utilized by stakeholders and external laboratories for pre-market
supervision of cosmetic products to ensure product quality and safety.

4. Conclusion
The analytical method for determining 1,4-Dioxane levels in cosmetics by GCMS-HSS
developed by CNQLDF has been collaborated and harmonized at the regional level into
ACM 011 and in the process of harmonization at the national level into INS. With the
harmonization of this method, all cosmetics laboratories in Indonesia and ASEAN,
including those incorporated in JLKI, have standardized analytical methods for testing 1,4
Dioxane to strengthen pre-market supervision of cosmetic products in ensuring product
quality and safety.
Acknowledgments
The authors are grateful to the Indonesian FDA, especially the Centre of National
Quality Laboratory of Drugs and Food (CNQLDF), which has provided research facilities,
funding, and support for conducting research.
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Strengthening the Surveillance of 1,4-Dioxane Contaminants in Cosmetics through Harmonization of
Analysis Methods and Networking of Cosmetics Laboratories in Indonesia
 ERUDITIO Vol. 4, No. 2, Juni 2024
P-ISSN: 2580-7722 | E-ISSN: 2807-6222

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Erita Lusianti, Yustina Yustina
Strengthening the Surveillance of 1,4-Dioxane Contaminants in Cosmetics through Harmonization of
Analysis Methods and Networking of Cosmetics Laboratories in Indonesia