色谱2016，Vol.34Issue(3)：249-257,9.DOI:10.3724/SP.J.1123.2015.10044
在线固相萃取结合液相色谱-线性离子阱多级质谱法同时检测生物样品中7种乌头类生物碱
Simultaneous determination of seven aconitum alkaloids in biological samples by liquid chromatography-linear ion trap multistage mass spectrometry coupled with on-line solid phase extraction
朱定姬 1黄晓青 2卢敏萍 3黄克建 2周哲 4林翠梧 3杨宁 2刘晓锋 2乔文涛 2李璐2
作者信息
- 1. 广西壮族自治区职业病防治研究院，广西 南宁 530021
- 2. 广西壮族自治区公安厅物证鉴定中心，广西 南宁 530012
- 3. 广西大学化学化工学院，广西 南宁 530004
- 4. 赛默飞世尔科技 中国 有限公司，上海 201206
- 折叠
摘要
Abstract
An analytical method has been developed for the simultaneous determination of seven aconitum alkaloids in biological samples by liquid chromatography-linear ion trap multistage mass spectrometry(LC-LIT/MSn)coupled with on-line solid phase extraction(on-line SPE). Mass fragmentation regularities of the seven aconitum alkaloids are discussed and summarized according to the analysis of their MS n fragments. The samples were treated with acetonitrile for protein precipitation,followed by dilution and centrifugation. The resulting solution was injec-ted into the LC system directly and processed by Waters Oasis ® HLB on-line SPE column for enrichment and purification. Chromatographic separation was performed on an Accucore C18 column using mobile phases of 0. 01 mol/L ammonium acetate aqueous solution and methanol (both containing 0. 1%(v/v)formic acid)for gradient elution. The analytes were detected in consecutive reaction monitoring( CRM)mode through positive electrospray ionization( ESI﹢). The calibration curves of the analytes within the investigated mass concentration ranges were fitted by second-order equations weighted 1/x,with r2 ranging from 0. 999 1 to 0. 999 9. The method detection limits were 0. 02-0. 60 ng/mL for whole blood and urine,0. 02-0. 40 ng/g for liver tissue. The recoveries at three spiked levels were within 91. 1%-104. 7% for all the ana-lytes,with 0. 2%-10. 7% of intra-day RSDs and 1. 0%-13. 7% of inter-day RSDs( n=6 ). The established method is simple,accurate,and sensitive for rapid determination of the seven aco-nitum alkaloids in biological samples.关键词
在线固相萃取/液相色谱-线性离子阱多级质谱法/连续反应监测/乌头类生物碱/生物样品Key words
on-line solid phase extraction( on-line SPE )/liquid chromatography-linear ion trap multistage mass spectrometry(LC-LIT/MSn)/consecutive reaction monitoring(CRM)/aconitum alkaloids/biological samples分类
化学化工引用本文复制引用
朱定姬,黄晓青,卢敏萍,黄克建,周哲,林翠梧,杨宁,刘晓锋,乔文涛,李璐..在线固相萃取结合液相色谱-线性离子阱多级质谱法同时检测生物样品中7种乌头类生物碱[J].色谱,2016,34(3):249-257,9.
