UPLC-MS/MS法测定人血浆中唑吡坦、扎来普隆及佐匹克隆的浓度

Determination of zolpidem tartrate,zaleplon and zopiclone in human plasma by UPLC-MS/MS

目的建立超高效液相色谱-串联质谱(UPLC-MS/MS)法测定人血浆中唑吡坦、扎来普隆及佐匹克隆的浓度。方法血样用乙酸乙酯进行萃取。色谱柱:Waters Acquity UPLC HSS T3(1.8μm,2.1 mm×100 mm),流动相:乙腈-0.1%甲酸水溶液,梯度洗脱,流速为0.3 mL·min-1,电喷雾离子源(ESI),正离子模式,多重反应监测(MRM)进行检测。结果唑吡坦、扎来普隆、佐匹克隆标准曲线方程分别为y=5.21x+0.14,y=1.61x+0.04,y=0.32x+0.02,相关系数均大于0.998,定量下限分别为0.02,0.04,0.04 ng·mL-1。3种被分析物的日内、日间RSD均小于15.3%。结论该方法快速、灵敏、准确,适用于人血浆中唑吡坦、扎来普隆及佐匹克隆的同时检测,可用于临床血药浓度检测。

Objective To develop a rapid ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)for determination of zolpidem tartrate,zaleplon,zopiclone(3-z drugs)in human plasma.Methods The plasma samples were extracted with acetoacetate.The separation was performed on a Waters Acquity UPLC HSST3 column(1.8μm,2.1 mm×100 mm)using the mobile phase composed of acetonitrile-0.1%formic acid solution at a flow rate of 0.3mL·min-1 in gradient elution mode.The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring(MRM)via electrospray ionization(ESI)source in positive mode.Results The calibration curves were y=5.21x+0.14,y=1.61x+0.04,y=0.32x+0.02 for zolpidem tartrate,zaleplon,zopiclone respectively.Good linear relation were obtained over the investigated concentration range,with all correlation coefficients higher than 0.998.The intra-and inter-day precision were all less than 15.3%.Conclusion The method was rapid,sensitive and reliable,and suitable for the simultaneous determination of 3-z drugs in human plasma in clinical.