反相液相色谱法测定片剂中噻马唑的含量

K. Poturcu, E. Demiralay
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摘要

本研究采用反相液相色谱法(RPLC)测定噻马唑(甲巯咪唑)在片剂中的含量。色谱柱为YMC Triart C18 (150 mm × 4.6 mm, 3μm, YMC, USA)。以pH 9.5的5% (v/v)乙腈-水二元混合物为流动相。选择甲硝唑作为内标。色谱分离流速0.8 ml/min,柱温25℃。噻唑和甲硝唑的波长分别为260 nm和340 nm。该方法在准确度、精密度、线性度、检出限(LOD)和定量限(LOQ)等方面进行了验证。在4 ppm ~ 14 ppm范围内,噻马唑的校准曲线呈线性关系。含5 mg噻马唑市售片(甲状腺马唑)的回收率为100.059%。该方法可用于商业片剂中噻马唑的含量测定。
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DETERMINATION OF THIAMAZOLE IN TABLET FORMULATION BY USING REVERSED PHASE LIQUID CHROMATOGRAPHIC METHOD
In this study, the amount of thiamazole (methimazole) in pharmaceutical tablet formulation was determined by using reversed phase liquid chromatography method (RPLC). Chromatographic separation was carried out by using YMC Triart C18 (150 mm × 4.6 mm, 3μm, YMC, USA) column. 5% (v/v) acetonitrile-water binary mixture at pH 9.5 was used as a mobile phase. Metronidazole was chosen as an internal standard. Flow rate was 0.8 ml/min and column temperature was 25 °C in chromatographic separation. The studied wavelengths for thiamazole and metronidazole are 260 and 340 nm, respectively. This proposed method was suitably validated with respect to accuracy, precision, linearity, the limit of detection (LOD) and limit of quantification (LOQ). The calibration graph of thiamazole was linear from 4 ppm to 14 ppm. The recovery of the 5 mg thiamazole containing commercial tablet (Thyromazol) was 100.059%. The proposed RPLC method was successfully applied to the determination of thiamazole in commercial tablet formulation.
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