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Abstract
Resorcinol is often misused for antiacne cosmetics. Corresponding to Indonesian FDA regulation, it is only allowed for hair dyes, hair lotion, and shampoo. Reference standard and analytical method of Resorcinol are needed for strengthening capability and capacity of Indonesian FDA for post-market controlling of cosmetics in Indonesia. Therefore, this research developed a reference standard by study and characterization and an analytical method for assay Resorcinol in raw material. Characterization of Resorcinol raw material using infrared spectrophotometry and HPLC-PDA, purity testing with TLC, HPLC, and DSC, homogeneity testing and assay by HPLC-PDA. Development analytical method for assay of Resorcinol was performed using an HPLC - PDA system with Waters Atlantis T3-C18 (5µm, 250 x 4.6 mm) column. The column temperature was set at 25°C. The mobile phase consists of ortho-phosphoric acid 0.085% pH 3 and methanol (50:50 v/v), delivered at a 1.0 mL/min flow rate. Detection was carried out at 274 nm. Resorcinol characterization using infrared spectrophotometry showed the presence of aromatic C-H bond functional groups (3100 – 3000 cm-1), C-H bonds (1374 and 773 cm-1), C-OH bonds (1311-1298, 1166; 1151 and 460 cm-1), C-C bonds (1608 and 1490 cm-1), aromatic rings (543 cm-1), and meta di-substituted ring groups (842 and 739 cm-1). Purity testing by TLC and HPLC were obtained that no spots or other peaks detected, indicating that the material has high purity. Purity by DSC of 99.05% and melting point of 109.41°C. The sample was homogenous with a content of 99.28% on a dried basis. Furthermore, the developed method has a linear range of 0.1 – 0.3 mg/mL at a coefficient correlation of 0.9999 and Vx0 of 0.5%. The limit of detection is 0.11 µg/mL, while the limit of quantification is 0.34 µg/mL and accuracy (% bias) of 0.10%. All validation parameters have met the requirement. These results meet the criteria for the candidate of a reference standard and the developed method is accurate, reliable, and valid so it can be applied to determine Resorcinol in raw material.
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References
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References
Ahuja, S. (2005). Overview: Handbook of pharmaceutical analysis by HPLC. In Separation Science and Technology (Vol. 6, Issue C). https://doi.org/10.1016/S0149-6395(05)80045-5
AOAC. (2002). AOAC Guidelines for Single Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals. AOAC.
Bernauer, U., Bodin, L., Commission, A. E., Chaudhry, Q., & Dusinska, M. (2021). SCCS Opinion on Resorcinol- SCCS / 1619 / 20 - Final Opinion Scientific Committee on Consumer Safety SCCS Opinion on Resorcinol The SCCS adopted this document. April.
BPOM. (2008). Peraturan Kepala BPOM No. HK.00.05.42.1018 tentang Bahan Kosmetik.
De, A. K., Chowdhury, P. P., & Chattapadhyay, S. (2014). Quantitative Analysis of Resorcinol from Marketed Hair Tonic Using Liquid Chromatographic Technique. International Scholarly Research Notices, 2014, 1 5. https://doi.org/10.1155/2014/632591
Goebel, C., Diepgen, T. L., Krasteva, M., Schlatter, H., Nicolas, J., Blömeke, B., Jan, P., Schnuch, A., Taylor, J. S., Pungier, J., Fautz, R., Fuchs, A., Schuh, W., Gerberick, G. F., & Kimber, I. (2012). Quantitative risk assessment for skin sensitisation : Consideration of a simplified approach for hair dye ingredients. Regulatory Toxicology and Pharmacology, 64(3), 459 465. https://doi.org/10.1016/j.yrtph.2012.10.004
Hahn, S., Kielhorn, J., Koppenhöfer, J., Wibbertmann, A., & Mangelsdorf, I. (2006). Concise international chemical assessment document 71. In IPCS Concise International Chemical Assessment Documents (Numéro 71).
ICH. (2005). Validation of Analytical Procedures : Text and Methodology Q2(R1). ICH Harmonised Tripartite Guideline, 1 13. https://doi.org/10.1002/9781118532331.ch23
ISO. (2017). ISO Guide 35 : Reference materials — Guidance for characterization and assessment of homogeneity and stability.
Kementerian Kesehatan Republik Indonesia, 2014, Farmakope Indonesia V hal. 1669-1673, Ketentuan Umum <1381> Validasi Prosedur dalam Farmakope, Jakarta: Kementerian Kesehatan Republik Indonesia.
Kosela, S. (2010). Cara Mudah dan Sederhana Penentuan Struktur Molekul berdasarkan Spectra Data (NMR, Mass, IR, UV). Lembaga Penerbit Fakultas Ekonomi UI.
Kumar Trivedi, M., & Branton, A. (2015). Characterisation of Physical, Spectral and Thermal Properties of Biofield treated Resorcinol. Organic Chemistry: Current Research, 04(03). https://doi.org/10.4172/2161-0401.1000146
Linsinger, T. P. J., Pauwels, J., Van Der Veen, A. M. H., Schimmel, H., & Lamberty, A. (2001). Homogeneity and stability of reference materials. Accreditation and Quality Assurance, 6(1), 20 25. https://doi.org/10.1007/s007690000261
Moffat, A. C., Osselton, M. D., Widdop, B., & Watts, J. (2004). Clarke’s Analysis of Drugs and Poisons (3rd éd.). Pharmaceutical Press.
Reynolds, J. E. F. (Éd.). (1982). Martindale: The Complete Drug Reference (28th éd.). Pharmaceutical Press.
Schmiedel, K., & Decker, D. (2000). Resorcinol. In Ullmann’s encyclopedia of industrial chemistry. Wiley-VCH, Weinheim.
Siti Maysarah, & Netti Herlina. (2015). Pembuatan Perekat Lignin Resorsinol Formaldehid Dari Natrium Lignosulfonat Tandan Kosong Kelapa Sawit. Jurnal Teknik Kimia USU, 4(4), 58 63. https://doi.org/10.32734/jtk.v4i4.1514
The United States Pharmacopeial. (2019). United State Pharmacopoeia 2019 USP 42- NF 37. In The United States Pharmacopeial Convention (Ed.), United State Pharmacopoeia 2019 USP 42- NF 37. The United States Pharmacopeia (USP).
The United States Pharmacopeial. (2020). United State Pharmacopoeia 2020 USP 43-NF 38. In United State Pharmacopoeia (Ed.), United State Pharmacopoeia (42nd-NF 38th ed.). United State Pharmacopoeia.
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.
Williams, M. (2013). The Merck Index: An Encyclopedia of Chemicals, Drugs, and Biologicals, 15th Edition Edited by M.J.O’Neil, Royal Society of Chemistry, Cambridge, UK ISBN 9781849736701; 2708 pages. April 2013, $150 with 1-year free access to The Merck Index Online. Drug Development Research, 74(5), 339 339. https://doi.org/10.1002/ddr.21085