液质联用法测定联用阿兹夫定前后人尿液中依非韦伦浓度  

Determination of efavirenz in healthy volunteer’s urine before and after co-administration with azvudine by HPLC-MS/MS

作　　者：刘冰洁 李青[1] 张西军[1] 常俊标 Liu Bingjie;Li Qing;Zhang Xijun;Chang Junbiao(National Demonstration Center for Experimental Chemistry Education,Henan Normal University,Xinxiang 453007,China;School of Chemistry and Chemical Engineering,Henan Normal University,Xinxiang 453007,China)

机构地区：[1]河南师范大学化学国家级实验教学示范中心,河南新乡453007 [2]河南师范大学化学化工学院,河南新乡453007

出　　处：《河南师范大学学报（自然科学版）》2020年第2期80-86,共7页Journal of Henan Normal University(Natural Science Edition)

基　　金：NSFC-河南联合基金(U1804283)。

摘　　要：建立液质联用法(HPLC-MS/MS)测定联用阿兹夫定(FNC)前后健康人尿液中的依非韦伦(EFV)浓度,为个体化治疗提供依据.色谱柱为Hypersil GOLD C18(2.1 mm×100 mm,3μm),流动相为2 mmol/L乙酸铵水溶液和甲醇,流速为0.2 mL/min,柱温30℃,进样量10μL,梯度洗脱,质谱采用电喷雾(ESI)电离正离子模式下的选择反应检测扫描(SRM),测定12例志愿者.EFV保留时间为7.1 min,线性范围为1~200 ng/mL,在该线性范围内标准曲线的相关性系数r^2>0.99.EFV连续单用14 d和联用FNC的7 d前后,EFV尿药浓度和排泄量无明显变化.该方法没有明显基质效应,能满足尿药研究需要,灵敏度高、准确性好.EFV和FNC联用对EFV的尿样排泄无显著影响.To establish an HPLC-MS/MS method for determining the concentration of efavirenz in healthy volunteer’s urine before and after co-administration with Azvudine(FNC).The HPLC procedure was performed on the Hypersil GOLD C18(2.1 mm×100 mm,3 μm),with the mobile phase composed of methanol and ammonium acetate solution(2 mmol/L),at the flow rate of 0.2 mL/min,colum temperature was 30 ℃,the injection volume was 10 μL,gradient elution method was used for HPLC and SRM scanning in positive ESI ionization mode was used for mass spectrometry in the determination of the 12 volunteers.The EFV’s retention time was 7.1 min,with a linearity range of 1-200 ng/mL the standard curve’s equation was established,r^2>0.99.The concentration and excretion of EFV in urine showed no significant change after 14 consecutive days of single-use EFV and 7 consecutive days of EFV combined with FNC.This determination method with small matrix effect is sensitive,accurate,and reliable,could be used to detect the concentration of EFV in urine.The co-administration of EFV and FNC had no significant effect on the excretion of EFV in urine.

关 键 词：依非韦伦 阿兹夫定 药物相互作用 HPLC-MS/MS 

分 类 号：O656.3[理学—分析化学]