Validasi Metoda Analisis Penetapan Kadar Ketoprofen pada Tablet Salut Enterik secara Kromatografi Cair Kinerja Tinggi dan Spektrofotometri UV

Salman Umar, Saafrida Saafrida, Henny Lucida

Abstrak


Ketoprofen yang beredar di Indonesia sebagian besar dalam bentuk sediaan tablet salut enterik, tetapi metoda analisis untuk penetapan kadar dan uji disolusinya belum tersedia dalam farmakope.  Tujuan dari penelitian ini adalah  mengembangkan metode kromatografi cair kinerja tinggi (KCKT) dan spektrofotometri ultraviolet visibel (UV) untuk  melakukan analisis tablet salut enterik ketoprofen. Penetapan kadar  dan keseragaman kandungan ketoprofen tablet salut enterik ditentukan secara KCKT isokratik fase terbalik yang telah divalidasi menggunakan kolom reverse phase (RP-18 ) (250 x 4,6 mm) diameter partikel 5 µm, fase gerak metanol-dapar fosfat 13 mM pH 6,5 perbandingan 60:40 v/v, laju alir 1,0 mL/menit dan detektor UV 258 nm. Spesifisitas, linieritas, akurasi, dan presisi  memenuhi persyaratan International Conference on Harmonization (ICH). Metode KCKT memberikan lineritas yang sangat baik (r > 0,999) pada rentang konsentrasi 15 – 35 µg/mL, presisi dinyatakan dalam persen deviasi standar relative (% RSD <0,87) dan perolehan kembali yang baik (R> 99,97%). Metode KCKT lebih sensitif dibandingkan metode spektrofotometri UV, dengan nilai LOD masing-masing adalah 0,18 dan 0,67 µg/mL serta LOQ 1,20 dan 2,49 µg/mL.  Hasil validasi dan uji penetapan kadar ketoprofen pada tablet salut enterik dengan metode KCKT tidak berbeda nyata dibandingkan dengan metode spektrofotometri UV (P>0,05)


Kata Kunci


ketoprofen; kromatografi cair kinerja tinggi; validasi metoda ; tablet salut enterik

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Referensi


E.Shohin I, Kulinich JI, Ramenskaya G V., Abrahamsson B, Kopp S. Biowaiver Monographs for Immediate-Release Solid Oral Dosage Forms: Ketoprofen. J Pharm Sci. 2012;101(7):2271–80. https://doi.org/10.1002/jps

BPOM RI: Cek Produk BPOM, [Online] [Accessed 22 juni 2020]. https://cekbpom.pom.go.id/home/produk

Matsui H., Shimokawa o., Kaneko T., Nagano Y., Rai K., Hyodo I. The pathophysiology of non-steroidal anti-inflammatory drug (NSAID)-induced mucosal injuries in stomach and small intestine. J Clin Biochem Nutr. 2011;48(2):7–111. doi:10.3164/jcbn. 10-79

Kulkarni R, Sa B. Enteric delivery of ketoprofen through functionally modified poly(acrylamide-grafted-xanthan)-based pH-sensitive hyd-rogel beads: Preparation, in vitro and in vivo evaluation., J Drug Target., 2008;16(2):167–77. https://doi.org/10.1080/1061186070179 2399M

Arida AI, Al-Tabakha MM. Encapsulation of ketoprofen for controlled drug release. European Journal of Pharmaceutics and Biopharmaceutics, 2007;66(1):48–54. https://doi.org/10.1016/j.ejpb. 2006.09.010

USP, The United States Pharmacopeia : the National Formulary (USP39-NF34). Easton: Mack Publishing Co; 2016.

FDA, SUPAC-MR : Modified Release Solid Oral Dosage Forms. Scale-Up and Post Approval Changes: Chemistry, Manufacturing, and Controls; In Vitro Dissolution Testing and In Vivo Bioequivalence Documentation. Washington,DC, U.S. Government Printing Office; 1997.

Menkes RI, Farmakope Indonesia (ed.V), Jakarta: Departemen Kesehatan RI; 2014.

BP, British Pharmacopoeia (B.P.). London, UK: The Stationery Office on behalf of the Medicines and Healthcare products Regulatory Agency (MHRA); 2017.

De Melo J, Hurtado FK, Prado AW, Souza MJE, Rolim CMB. Validation of HPLC and UV spectrophotometric methods for the determination of bezafibrate in pharmaceutical formulations. J Liq Chromatogr Relat Technol. 2008;31(2):269–80. https://doi.org/10.1080/10826070701739108

Bajaj, S., Singla, D., &, Sakhuja, N. Stability testing of pharmaceutical products. Journal of applied pharmaceutical science, 2012;2(3),129-138. https://doi.org/10.7324/JAPS.2012.2322

El-Saharty, Y. S., Metwally, F. H., Refaat, M., & El-Khateeb, S. Z. Simultaneous Determination of Hyoscine Butylbromide and Ketoprofen in Pharmaceutical Preparations by Spectrophotometric and Liquid Chromatographic Methods, Journal of AOAC International, 2007;90(1):102-112., https://doi.org/10.1093/jaoac/90.1.102

Özlü C, Basan H, Şatana E, Ertaş N, Göǧer NG., Quantitative determination of ketoprofen in gels and ampules by using flow-injection UV spectrophotometry and HPLC: Journal of Pharmaceutical and Biomedical Analysis; 2005,39 (3–4): 606–11. https://doi.org/10.1016/j.jpba.2005.04.002

Blanco, M., González, J., Torras, E., & Valverde, I. Enantiomeric purity determination of ketoprofen by capillary electrophoresis: development and validation of the method. Analytical and bioanalytical chemistry. 2003,375(1):157–163. https://doi.org/10.1007 /s00216-002-1629-8

Dvořák, J., Hajkova, R., Matysova, L., Novakova, L., Koupparis, M. A., & Solich, P.,Simultaneous HPLC determination of ketoprofen and its degradation products in the presence of preservatives in pharmaceuticals.: Journal of pharmaceutical and biomedical analysis. 2004;36(3),625-629., https://doi.org/10.1016/j.jpba.2004.07.018.

Bempong, D. K. & Bhattacharyya, L., Development and validation of a stability-indicating high-performa liquid chromatographic assay for ketoprofen topical penetrating gel.: Journal of Chromatography A. 2005;1073(1-2),341-346. https://doi.org/10.1016/j.chroma.2004.12.061

Yadav, N. K., Raghuvanshi, A., Sharma, G., Beg, S., Katare, O. P., & Nanda, S, QbD-based development and validation of a stability-indicating HPLC method for estimating ketoprofen in bulk drug and proniosomal vesicular system.: Journal of Chromatographic Science. 2016;54(3),377-389., https://doi.org/10.1093/chromsci/bmv151

Parmar, A. & Sharma, S., Derivative UV-vis absorption spectra as an invigorated spectrophotometric method for spectral resolution and quantitative analysis: Theoretical aspects and analytical applications: A review.. TrAC Trends in Analytical Chemistry. 2016;77, 44-53. https://doi.org/10.1016/j.trac.2015.12.004

Mendez, A.S.S.M. &. S.E., Validation of HPLC and UV spectrophotometric methods for the determination of meropenem in pharmaceutical dosage form. Journal of pharmaceutical and biomedical analysis. 2003;33(5),947-954. https://doi.org/10.1016/ S0731-7085(03)00366-2

Ahuja, S., & Rasmussen, H, eds. HPLC method development for pharmaceuticals.. Amterdam, Netherlands: Elsevier, 2011.

Dagron S. Die International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH). Handb Ethik und R der Forsch am Menschen. 2014;541–5. https://doi.org/10.1007/9783642-35099-3_86




DOI: https://doi.org/10.25077/jsfk.8.2.200-207.2021

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