LC-MS/MS法快速测定吡罗昔康制剂中吡罗昔康含量

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。

Rapid quantification of piroxicam in piroxicam preparations by using LC-MS/MS

An improved method was developed for the quantification of piroxicam in piroxicam preparation by ultra fast liquid chromatography/tandem mass spectrometry(LC/MS/MS).METHOD Sample preparation consisted of extraction by adding 0.1 mol/L hydrochloric acid in methanol,filtration with microporous membrane and centrifugation of the sample subsequently.LC/MS/MS detection was performed by using a triple-stage quadrupole mass spectrometer working in multiple reaction monitoring mode(MRM) with positive electrospray ionization(ESI),using the transitions of m/z 332.2→94.8 of piroxicam.Chromatographic separation was achieved using a 3.0mm×75mm,2.0 μm Shim-pack XR-ODS column with isocratic flow and elution with acetonitrile-water-formic acid(60:40:0.1,V/V/V) and a flow-rate of 0.4 mL/min.The analyte was quantified in a single run within 3 min.RESULTS Linearity was demonstrated over the expected concentration range of 2.5~1000.0 ng/mL.The lower limit of quantification(LLOQ) was 2.5 ng/μmL.Intra-day precision expressed as RSD was less than 3.2%,while inter-day result was less than 3.8% for piroxicam.CONCLUSION The method has good repeatability,high sensitivity and more convenient,and can be successfully applied to the determination of piroxicam in piroxicam preparations.The described method is also suitable to for analysies of serum samples with very small volumes and for pharmacokinetic studies.