Karakterisasi dan Pengembangan Metode Analisis Kromatografi Cair Kinerja Tinggi (KCKT) untuk Penetapan Kadar Asam Glikolat sebagai Calon Baku Pembanding

Dila kartika Aprianti; Neni Isnaeni

doi:10.69606/jcse.v3i01.450

Authors

Dila kartika Aprianti BPOM
Neni Isnaeni BPOM

DOI:

https://doi.org/10.69606/jcse.v3i01.450

Keywords:

Glycolic acid, characterization, assay, reference standard, HPLC

Abstract

Glycolic acid is a widely used peeling agent in skincare cosmetics that is effective in treating hyperpigmentation, wrinkles, and acne scars. However, due to its potential to cause irritation and erythema, the concentration of this substance in cosmetic products must be strictly controlled. This study aimed to develop an analytical method and to establish a reference value for glycolic acid in order to enhance laboratory testing capabilities for the regulatory surveillance of cosmetic products in the community. Raw material characterization was carried out using infrared spectrophotometry and High-Performance Liquid Chromatography (HPLC). Purity testing was performed using Differential Scanning Calorimetry (DSC) and HPLC, while water content was determined by coulometric analysis. Homogeneity testing and assignment of the content (assigned value) were conducted using an HPLC–PDA system equipped with an autosampler and a C18 column (250 × 4.6 mm i.d., 5 µm). The mobile phase consisted of 15% methanol (pH 2 adjusted with 85% orthophosphoric acid). The results showed that the raw material purity determined by DSC was 98.06% with a melting point of 74.15 °C, while HPLC purity testing detected a total impurity level of 0.40%. The water content of the raw material was recorded at 0.62%. Statistical analysis confirmed that the material was homogeneous, as indicated by an F calculated value lower than the F table value (1.97 < 3.02). Using this method, the assigned value of glycolic acid content was determined to be 98.98% with an associated uncertainty (U) of 1.54%. All validation parameters of the developed analytical method met the acceptance criteria, demonstrating that the HPLC–PDA method is accurate and valid for the determination of glycolic acid content. Based on the purity profile, homogeneity, and assigned value obtained, this raw material is legitimate and suitable for use as a glycolic acid reference standard in cosmetic testing.

References

Alauhdin, M., Edan, W.T., & Alighiri, D. (2021). Aplikasi Spektroskopi Inframerah untuk Analisis Tanaman dan Obat Herbal. Universitas Negeri Semarang. Doi:https://doi.org/10.15294/.v0i0.15

BPOM. (2024). Peraturan Badan Pengawas Obat Dan Makanan Nomor 18 Tahun 2024 Tentang Penandaan, Promosi, Dan Iklan Kosmetik

BPOM. (2019). Peraturan Badan Pengawas Obat Dan Makanan Nomor 23 Tahun 2019 Tentang Persyaratan Teknis Bahan Kosmetika.

Gill, Pooria., Moghadam, T.T., & Ranjbar, B. (2010). Differential Scanning Calorimetry Techniques: Applications in Biology and Nanoscience. Journal of Biomolecular Techniques, 21, 167–193.

ISO. (2017). ISO Guide 35 : Reference materials — Guidance for characterization and assessment of homogeneity and stability.

Jarukas L, et.al. (2020). Investigation of Organic Acids in Sa ron Stigmas (Crocus sativus L.) Extract by Derivatization Method and Determination by GC/MS. Molecules, 25, 3427. doi:10.3390/molecules25153427

Kementerian Kesehatan Republik Indonesia, 2020, Farmakope Indonesia VI hal. 2165, Prosedur Disolusi: Pengembangan Dan Validasi <1353>. Jakarta: Kementerian Kesehatan Republik Indonesia.

Narda, M., et.al. (2020). Glycolic acid adjusted to pH 4 stimulates collagen production and epidermal renewal without affecting levels of proinflammatory TNF-alpha in human skin explants. Journal of Cosmetic Dermatology, 20, 513-521. DOI: 10.1111/jocd.13570

Nurhamidah, W., et al., (2024). Aplikasi Penggunaan Spektroskopi Infrared dan Spektrofotometri UV-Vis Dalam Identifikasi Senyawa Bioaktif Ekstrak Tumbuhan: Literature Review Article. Journal Of Social Science Research, 4(1), 3612-3622.

Pastuszak, D.O., et.al. (2025). Application of Karl Fischer titration method to determine moisture content of building materials. https://doi.org/10.1016/j.measurement.2025.118363.

Shahbano., et.al. (2023). Comparison of effectiveness and safety of 35% glycolic acid peel with microneedling versus glycolic acid peel alone in the management of acne scars. Journal of Pakistan Association of Dermatologists, 33(2), 608-613.

Sharad, J. (2013). Glycolic acid peel therapy – a current review. Clinical, Cosmetic and Investigational Dermatology, 6, 281-288.

The United States Pharmacopeial. (2011). First Supplement to USP 40 - NF 35 <621> Chromatography. In The United States Pharmacopeial Convention (Ed.), United State Pharmacopoeia 2019 USP 42- NF 37. The United States Pharmacopeia (USP).

Verma, A., et.al. (2018). Mechanistic Aspect of Iridium(III) Catalyzed Oxidation of Ethylene Glycol by Chloramine-T in Aqueous Acidic Medium: A Kinetic Model. International Journal of Chemical and Physical Sciences, 7(1). 62-71. DOI:10.30731/ijcps.7.1.2018.62-71

WHO. (2007). WHO committee on specifications for pharmaceutical preparations, Annex 3, general guidelines for the establishment, maintenance, and distribution of chemical reference standards. Geneva: WHO.

Wignjosoesastro, T.S., Widyawati., Sugianto, R. (2021). The Effect Of Glycolic Acid And Vitamin C Topical In Freckles Efficacy. Jurnal Kedokteran Diponegoro, 10(1).