杨汉煜,陈笑艳,徐海燕,侯悦,钟大放
YANG Han yu;CHEN Xiao yan;XU Hai yan;HOU Yue;ZHONG Da fang (Laboratory of Drug Metabolism and Pharmacokinetics;

• 1:沈阳药科大学药物代谢与药物动力学实验室!辽宁沈阳110016
• 2:沈阳药科大学药物代谢与药物动力学实验室!辽宁沈阳110016
• 3:沈阳药科大学药物代谢与药物动力学实验室!辽宁沈阳110016
• 4:沈阳药科大学药物代谢与药物动力学实验室!辽宁沈阳110016

摘要(Abstract)：

建立了测定人血浆中伪麻黄碱浓度的液相色谱 串联质谱法。血浆样品经液 液萃取处理后 ,以甲醇 水 甲酸 (体积比 6 0∶40∶2 )为流动相 ,采用ZorbaxC18柱分离 ,通过电喷雾四极杆串联质谱 ,正离子方式检测 ;采用SRM转化m/z 16 6→ 147(伪麻黄碱 )和m/z 2 75→ 12 5 (内标罗哌卡因 )进行定量分析。线性范围为 5 0～ 2 5 0 0ng/mL ,定量限为 5 0ng/mL。应用本法测试了 2 0名健康受试者口服 6 0mg盐酸伪麻黄碱后不同时刻的血浆药物浓度
A specific,sensitive and rapid LC/MS/MS method for determination of pseudoephedrine in the human plasma was developed. Pseudoephedrine and the internal standard ropivacaine were extracted from plasma using liquid liquid extraction,then separated on a Zorbax C 18 column. The mobile phase consisted of methanol water formic acid (60∶ 40∶ 2, V/V ),and was set at a flow rate of 0 2 mL/min. A Finnigan TSQ tandem mass spectrometer equipped with electrospray ionization source was used as the detector and was operated in the positive ion mode. Selected reaction monitoring (SRM) using the precursor→product ion combinations of m/z 166→147 and m/z 275→125 was used to quantify the pseudoephedrine and the internal standard,respectively. The linear calibration curves were obtained in the concentration range of 5 0～ 250 0 ng/mL . The limit of quantification was 5 0 ng/mL . Within day and between day precision were within 6 7% and 8 3%,respectively. The method was successfully applied to determining the concentrations of pseudoephedrine in human plasma after an oral administration of 60 mg pseudoephedrine hydrochloride to 20 healthy volunteers.

关键词(KeyWords)： 伪麻黄碱;液相色谱串联质谱法;血浆药物浓度
pseudoephedrine; liquid chromatography tandem mass spectrometry; plasma concentration

Abstract:

Keywords:

基金项目(Foundation): 国家自然科学基金资助项目!(39930 180 )

作者(Authors): 杨汉煜,陈笑艳,徐海燕,侯悦,钟大放
YANG Han yu;CHEN Xiao yan;XU Hai yan;HOU Yue;ZHONG Da fang (Laboratory of Drug Metabolism and Pharmacokinetics;

参考文献(References)：

• [1]BrendelE ,MeinekeI,HenneEM ,etal .Sensitivehigh performanceliquidchromatographicdeterminationofpseudoephedrineinplasmaandurine [J].JChromatogrB ,1988,42 6 :40 6～ 411.
• [2 ]NiederM ,JaegerH .Sensitivequantificationofpseu doephedrineinhumanplasmaandurinebyhigh perfor manceliquidchromatography [J].JChromatogrB ,1988,42 4:73～ 82 .
• [3]SunSY ,LevequeMJ .Electron captureGLCdetermi nationofpseudoephedrineinserum [J].JPharmSci,1979,6 8:15 6 8～ 15 6 9.
• [4 ]ChaoST ,PratherD ,PinsonD ,etal .Effectoffoodonbiovailabilityofpseudoephedrineandbrompheniramineadministeredfromagastrointestinaltherapeuticsystem[J].JPharmSci,1991,80 :432～ 435 .
• [5 ]杨丽莉 ,屠锡德 .气相色谱 质谱法测定血中伪麻黄碱[J].药学学报 .1993 ,2 8:70 9～ 713 .
• [6 ]钟大放 .以加权最小二乘法建立生物分析标准曲线的若干问题 [J].药物分析杂志 ,1996 ,16 :30 6～ 312 .
• [7]KarnesHT ,MarchC .Precision ,accuracy ,anddataac ceptancecriteriainbiopharmaceuticalanalysis [J].PharmRes ,1993 ,10 :142 0 .
• [8]中华人民共和国国家药典委员会 .中华人民共和国药典 :二部 .北京 :化学工业出版社 ,2 0 0 0 .