摘要
目的建立测定人体内红霉胺血药质量浓度的液相色谱-串联质谱法（LC-MS-MS），为地红霉素药物动力学研究提供方法学依据。方法待测血浆0．5mL用乙醚-二氯甲烷萃取。色谱柱：Zobax XDB C18柱；流动相：甲醇-水-甲酸（体积比80：20：0．5）；流速：0.6mL·min^-1。液相色肾串联质谱采用多反应离子检测，正离子模式。结果血浆中无干扰测定的内源性物质；每个样品分析时间小于4min；线性范围为1．0～1000μg·L^-1，定量下限为1．0μg·L^-1；批内、批间精密度均小于15％。结论LC-MS-MS法可用于红霉胺的临床药物动力学研究。
Objective To develop a sensitive and specific liquid chromatography-tandem mass spectrometry （LC-MS-MS） method for determination of erythromycylamine in human plasma. Methods Erythromycylamine was extracted by diethyl ether and dichloromethane from human plasma, and then separated on a C1s colunto. The mobile phase consisted of methanol-water-formic acid（ V： V： V = 80：20：0.5 ） and the flow rate was 0.6mL·min^-1. A mass spectrometer equipped with electrospray ionization source was used as detector and operated in the positive ion mode. In multiple reaction monitoring（MRM） mode ,the ion combination of m/z 749→m/z 591[M ＋ H]^＋ and m/z 748→m/z 158 [ M ＋ H]^＋ were used to quality erythromycylamine and an internal standard（ clarithromycin）, respectively. Results Chromatograms showed no endogenous interfering peaks in the respective blank human plasma samples. Each analysis was completed within 4 min. The calibra- tion was linear in the concentration range within 1. 0 - 1 000μg·L^-1 and quantitative limit was 1.0μg·L^-1. The intra-batch and inter-batch RSD were less than 15%. Conclusions The method is proved to be suitable for clinical investigation of erythromycylamine pharmacokinetics, which offers advantages of specificity, quickness and higher sensitivity over the previously reported methods.
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2009年第5期393-396,共4页
Journal of Shenyang Pharmaceutical University
关键词
地红霉素
红霉胺
液相色谱-串联质谱法
血浆浓度
含量测定
dirithromycin
erythromycylamine
liquid chromatography-tandem mass spectrometry（ LC-MS- MS）
plasma concentration
content determination
