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高效液相色谱-电喷雾电离串联质谱法同时测定体液中的五种有毒生物碱

Simultaneous determination of five toxic alkaloids in body fluids by high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry.

作者信息

Qiu Peihong, Chen Xiaohong, Chen Xiang, Lin Li, Ai Changchun

机构信息

School of Pharmacy, Wenzhou Medical College, Wenzhou, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Nov 15;875(2):471-7. doi: 10.1016/j.jchromb.2008.09.034. Epub 2008 Oct 2.

Abstract

A novel analytical method was developed and validated for the rapid and simultaneous analysis of five toxic alkaloids: Brucine, Strychnine, Ephedrine, Aconitine and Colchicine, in blood and urine using high-performance liquid chromatography-electrospray ionization tandem mass spectrometry in the multiple reaction monitoring (HPLC-ESI-MRM) mode. The linear range was 0.05-50.0 ng mL(-1) for Brucine, 0.1-50.0 ng mL(-1) for Strychnine and Ephedrine, 0.01-10.0 ng mL(-1) for Aconitine and Colchicine. The limits of quantification for Brucine, Strychnine, Ephedrine, Aconitine and Colchicine were found to be 0.03, 0.05, 0.20, 0.05, 0.01 ng mL(-1), respectively. The average extraction recoveries in urine ranged from 96.0 to 114.0% and in whole blood were 94.0 to 113.0%. The intra-day and inter-day RSDs were less than 8.3 and 10.6%, respectively. The five alkaloids could be well separated within 7 min in a single run. The established method should be suitable for the determination of trace alkaloids in body fluids.

摘要

建立并验证了一种新型分析方法,该方法采用高效液相色谱-电喷雾电离串联质谱的多反应监测(HPLC-ESI-MRM)模式,可快速同时分析血液和尿液中的五种有毒生物碱:马钱子碱、士的宁、麻黄碱、乌头碱和秋水仙碱。马钱子碱的线性范围为0.05 - 50.0 ng mL(-1),士的宁和麻黄碱为0.1 - 50.0 ng mL(-1),乌头碱和秋水仙碱为0.01 - 10.0 ng mL(-1)。马钱子碱、士的宁、麻黄碱、乌头碱和秋水仙碱的定量限分别为0.03、0.05、0.20、0.05、0.01 ng mL(-1)。尿液中的平均提取回收率为96.0%至114.0%,全血中的为94.0%至113.0%。日内和日间相对标准偏差分别小于8.3%和10.6%。这五种生物碱在一次进样中可在7分钟内很好地分离。所建立的方法应适用于体液中痕量生物碱的测定。

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