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建立了快速液相色谱-质谱/质谱联用法测定吡罗昔康制剂中吡罗昔康含量的方法。样品以0.1 mol/L盐酸甲醇溶液提取、微孔滤膜过滤、离心后,通过电喷雾离子化(ESI),采用多反应检测(MRM)方式进行正离子检测,用于定量分析的检测离子为m/z 332.2→94.8。采用Shim-pack XR-ODS(3.0 mm×75mm,2.0μm)柱分离,以乙腈-水-甲酸(60:40:0.1,V/V/V)为流动相,流速为0.40 mL/min,在3 min内完成吡罗昔康定量分析。线性范围为2.5～1000.0ng/mL,最低检测限为2.5 ng/mL;日内测定的相对标准偏差小于3.2%,日间测定的相对标准偏差小于3.8%。方法可作为吡罗昔康制剂的质量中吡罗昔康控制方法,并可用于少量血浆样品的测定,也适用于药物代谢动力学研究。
A rapid liquid chromatography-mass spectrometry / mass spectrometry method was established for the determination of piroxicam in piroxicam. The sample was extracted with 0.1 mol / L hydrochloric acid methanol solution, filtered through a microporous membrane filter, centrifuged, electrospray ionized (ESI) and multi-reaction detection (MRM) m / z 332.2 → 94.8. The column was separated on a Shim-pack XR-ODS (3.0 mm × 75 mm, 2.0 μm) column with acetonitrile-water-formic acid (60:40: 0.1, V / V / V) as the mobile phase at a flow rate of 0.40 mL / Piroxicam quantitative analysis was completed within 3 min. The linear range was 2.5-1000.0 ng / mL with the minimum detectable limit of 2.5 ng / mL. The relative standard deviations (RSDs) were less than 3.2% and the relative standard deviations (RSDs) were less than 3.8%. The method can be used as a method for controlling the quality of piroxicam, and can be used for the determination of a small amount of plasma samples, and also for pharmacokinetic studies.