Validation of Analytical Method LC MS/MS for Determination Isoniazid in Rats Serum

Andi Suhendi(1*), Abdul Rohman(2), Djoko Wahyono(3), Arief Nurrochmad(4), Tasya Faradillah Manggo(5)

(1) Universitas Muhammadiyah Surakarta
(2) Pharmaceutical Chemistry Department, Faculty of Pharmacy, Universitas Gadjah Mada, Sekip, Sleman, Indonesia
(3) Pharmacology and Clinical Pharmacy Department, Faculty of Pharmacy, Universitas Gadjah Mada
(4) Pharmacology and Clinical Pharmacy Department, Faculty of Pharmacy, Universitas Gadjah Mada
(5) Pharmaceutical Chemistry Department, Faculty of Pharmacy, Universitas Muhammadiyah Surakarta
(*) Corresponding Author

Abstract

Determination of isoniazid concentration for therapeutic drug monitoring must produce valid values, so validation of the analytical method of LC-MS/MS needs to be carried out. This research aims to obtain valid method of LCMS/MS in order to determination isoniazid in rats serum. Sample preparation was carried out using the liquid-liquid extraction method using acetonitrile and methanol (2:1). The chromatography system was developed with a C18 column (ACQUITY UPLC® HSS T3 1.8 µm, 2.1 × 100 mm), the mobile phase was 70% acetonitrile with 0.1% formic acid (A), water with 0.1% formic acid (B), as well as methanol (C) with a flow rate of 0.3 mL/min, with gradient elution, detection in ESI+ mode with multiple reaction monitoring (MRM) at the transition 138 m/z → 121 m/z. The research results showed that the method was accurate with a % recovery of 96 - 113% and an RSD of 2.4 ± 0.9%. The precision value was obtained with an average RSD of 3.7 ± 2.4% for intra-day and 4.1 ± 2.3% for inter-day. Linearity showed good results with a correlation coefficient of 0.9956 in tests with 5 different concentrations. The LOQ and LOD values obtained from the linear regression equation were 0.1987 µg/mL and 0.0656 µg/mL respectively. The results showed that the LC-M/MS method was valid for determining isoniazid levels in rat serum

Keywords

validation, LCMS/MS, isoniazid, Multiple Reaction Monitoring (MRM), rats serum

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DOI: 10.23917/pharmacon.v20i2.23293

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