UPLC-MS/MS法同时测定人血浆中度洛西汀和劳拉西泮的浓度  

Simultaneous determination of dexmedetomidineanddezocine in humanplasma by HPLC-MS/MS

作　　者：贺利峰[1] 袁玉梅[2] 邱彩霞[1] 杨湘燕 HE Li-feng;YUAN Yu-mei;QIU Cai-xia;YANG Xiang-yan(Department of Neurology,Huzhou Central Hospital,Huzhou 313000,Zhejiang Province,China;Department of Pharmacy,Huzhou Central Hospital,Huzhou 313000,Zhejiang Province,China)

机构地区：[1]湖州市中心医院,神经内科,浙江湖州313000 [2]湖州市中心医院,药剂科,浙江湖州313000

出　　处：《中国临床药理学杂志》2021年第22期3153-3156,共4页The Chinese Journal of Clinical Pharmacology

摘　　要：目的建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定人血浆中度洛西汀和劳拉西泮的浓度。方法血浆样本用甲醇沉淀蛋白,以罗通定为内标,色谱柱:Zorbax EclipseXDB-C_(18)(2.1 mm×100.0 mm,3.5μm),流动相:10 mmol·L^(-1)乙酸铵溶液(含0.1%甲酸)-甲醇=62∶38,流速:0.2 mL·min^(-1),进样量:5.0μL。电喷雾离子源,多离子反应监测,正离子扫描。用于定量分析的离子对为度洛西汀(m/z 298.2→m/z 154.1)、劳拉西泮(m/z 321.0→m/z 275.1)和内标罗通定(m/z 356.2→m/z 192.2)。考察该方法的专属性、标准曲线和定量下限、精密度与回收率、基质效应及稳定性。结果度洛西汀在0.56~225.27 ng·mL^(-1)线性关系良好,标准曲线为y=0.12x-1.68×10^(-3)(R_(2)=0.9986),定量下限为0.56 ng·mL^(-1);劳拉西泮在0.51~204.20 ng·mL^(-1)线性关系良好,标准曲线为y=7.57×10^(-2) x+4.64×10^(-3)(R_(2)=0.9991),定量下限为0.51 ng·mL^(-1);度洛西汀和劳拉西泮的平均提取回收率在93%以上,日内和日间的精密度RSD均小于10%,基质不影响测定,样品的稳定性良好。结论本方法简便快速,准确度高,灵敏度好,适用于人血浆中度洛西汀和劳拉西泮的浓度测定。Objective To establish an UPLC-MS/MS method for the determination of duloxetine and lorazepam in human plasma.Methods Plasma samples were treated by the protein precipitation method with methanol as the internal standard using rotundine.Chromatographic separation was performed on a Zorbax Eclipse XDB-C_(18)(2.1 mm×100.0 mm,3.5μm).Mobile phase was 10 mmol·L^(-1) ammonium acetate solution(containing 0.1%formic acid)-methanol=62∶38.Flow rate was 0.2 mL·min^(-1).Injection volume was 5.0μL.MS detection was carried out using an electrospray ionization source operated in multiple reaction monitoring(MRM)mode.The MS/MS ion transitions monitored were m/z 298.2→m/z 154.1(duloxetine),m/z 321.0→m/z 275.1(lorazepam),m/z 356.2→m/z 192.2(rotundine).The specificity,standard curve,lower limit of quantification,precision,recovery,stability and matrix effect of the method were investigated.Results The calibration curves of duloxetine and lorazepam were y=0.12x-1.68×10^(-3)(R_(2)=0.9986)and y=7.57×10^(-2)x+4.64×10^(-3)(R_(2)=0.9991),with the linear ranges of 0.56-225.27 ng·mL^(-1) and 0.51-204.20 ng·mL^(-1),and the lower limits of quantification were 0.56 ng·mL^(-1) and 0.51 ng·mL^(-1),respectively.The average extraction recoveries of the two drugs were above 93%,and the standard deviations of intraday and daytime precision were less than 10%.The experiment has good stability and was not affected by matrix effect.Conclusion The method is simple,accurate and reliable,suitable for the determination of duloxetine and lorazepam in human plasma.

关 键 词：度洛西汀 劳拉西泮 血浆 超高效液相色谱-质谱 

分 类 号：R971[医药卫生—药品]