摘要
目的建立LC/MS/MS法测定人血浆中劳拉西泮含量的方法,研究其片剂生物等效性.方法取血浆样品0.3mL,加入内标地西泮乙腈溶液0.6mL,涡流混合5min,高速离心15min,取上清液20μL进样,流动相:0.04%甲酸-乙腈(35:65,V/V);流速: 0.2mL/min;ZORBAX Eclipse XDB- C18(2.1mm×100mm,3.5μm).采用电喷雾离子源三级四极杆串联质谱,以选择反应监测(SRM)方式进行检测.用于定量分析的离子反应分别为m/z 321→275(劳拉西泮) 和m/z 285 →193(内标:地西泮). 结果劳拉西泮线性范围为0.71~71.33ng·mL-1,定量限为0.71 ng·mL-1,三种浓度的相对回收率为108.8%~112.3%,日内、日间RSD均小于4.1%(n=5).结论本法专属、灵敏、快速,适用于劳拉西泮的生物等效性研究.
OBJECTIVE To establish a LC/MS/MS method for determination of lorazepam in plasma and to study its bioequivalence. METHODS 0.3mL of the plasma sample was pipetted into a conical tube, 0.6mL internal standard solution containing diazepam in acetonitrile was added, the mixture was agitated for 5 min using a vortex agitator and centrifuged for 15 min at high speed. Then 20μL of supernatant was injected into the chromatograph. The mobile phase consisted of 0.04% formic acid -acetonitrile(35: 65), the flow rate was 0.2mL · min^ -1, the column was ZORBAX Eclipse XDB- C18 (2.1 × 100mm,3.5 μm). Electrospray ionization source was applied and operated in positive ion mode. Selected reaction monitoring(SRM) mode with the transitions of m/z 321→275 and m/z 285→193 was used to quantify lorazepam and diazepam respectively. RESULTS The linear calibration curve was obtained in the range of 0.71 -71.33 ng · mL^-1 ,The lower limit of quantification was 0.71 ng · mL^-1 ,three level concentration relative recoveries were 108.8% - 112.3% ,the intra-day and inter-day precision (RSD) were below 4.1%. CONCLUSION The method is simple, rapid,accurate and can be used to study bioequivalence of lorazepam.
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2005年第4期318-321,共4页
Chinese Journal of Modern Applied Pharmacy
关键词
劳拉西泮
液相色谱-串联质谱法
生物等效性
lorazepam
liquid chrumatography-tandem mass spectrometry
bioequivalence