摘要
目的建立高效液相色谱质谱联用测定人血浆中氯唑沙宗及其代谢物6-羟基氯唑沙宗的方法。方法采用Thermo C18色谱柱（4.6 mm×150 mm,5μm）,Phenomenex C18保护柱,柱温40℃,流动相：乙腈-30 mmol·L^-1醋酸铵溶液（34∶66）,流速：1mL·min^-1,进入MS检测器的分流比3∶1。质谱采用电喷雾电离源负离子模式（ESI^-）,选择性监测质荷比（m/z）168.3,170.2（氯唑沙宗）,444.7（内标）,184.4,186.2（6-羟基氯唑沙宗）的准分子离子峰。血浆样品孵化后,经叔丁基甲醚提取,内标法定量。结果氯唑沙宗及6-羟基氯唑沙宗分别在25-10 000,10-3 000μg·L^-1内线性关系良好（r≥0.999 8）;最低检测质量浓度分别为2.5和2μg·L^-1;两个化合物的方法回收率在90%-110%之间;日间和日内RSD均小于15%。结论该方法灵敏度高,快速,简便,可用于氯唑沙宗药动学及药物相互作用的研究。
OBJECTIVE To establish a high performance liquid chromatography-electrospray mass spectrometry method for the determination of chlorzoxazone and its metabolite in human plasma. METHODS The HPLC separation was performed on a Thermo C18 column（4. 6 mm×150 mm,5μm） with guard column phenomenex C18 The column temperature was 40 ℃. The mobile phase consisted of acetonitrile -30 mmol · mL^-1 ammoniumacetate solution. The flow rate was 1 mL·min^-1 with a split ratio 3：1 . The compound was ionized in the electrospray ionization （ESI） negative ion source of mass spectrometer and selected ions were at m/z 168.3,170. 2 （CZX） ,444.7 （IS）and 184. 4,186. 2 （HCZX） . Human plasma samples were extracted with methyl t-butyl ether after incubation. RESULTS The linear ranges were 25 - 10 000 μg·L^-1 for chlorzoxazone, 10 - 3 000 μg·L^-1 for 6-hydroxychlorzoxazone （r≥0. 999 8） ,and their detect limits were 2. 5,2. 0 μg·L^-1 Recoveries were within 90% - 110%, and intra-and inter-day RSDs were all less than 15%. CONCLUSION The method appeared to be accurate,sensitive,specific and simple. It is suitable for clinical study of chlorzoxazone pharmacokinetics and drug interaction.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2007年第13期1011-1014,共4页
Chinese Pharmaceutical Journal
