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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
引用本文:朱定姬,卢敏萍,黄克建,周哲,林翠梧,杨宁,刘晓锋,乔文涛,李璐,黄晓青.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.
作者姓名:朱定姬  卢敏萍  黄克建  周哲  林翠梧  杨宁  刘晓锋  乔文涛  李璐  黄晓青
作者单位:1. 广西壮族自治区职业病防治研究院, 广西 南宁 530021; 2. 广西大学化学化工学院, 广西 南宁 530004; 3. 广西壮族自治区公安厅物证鉴定中心, 广西 南宁 530012; 4. 赛默飞世尔科技(中国)有限公司, 上海 201206
摘    要:建立了在线固相萃取(on-line SPE)结合液相色谱-线性离子阱多级质谱(LC-LIT/MSn)同时测定全血、尿液和肝组织样品中7种乌头类生物碱的分析方法,并根据7种乌头类生物碱的多级质谱碎片对裂解规律进行了推测和总结。用乙腈沉淀样品中的蛋白质,于稀释和离心后直接进样。经Waters Oasis® HLB在线SPE柱富集纯化,以0.1%(v/v)甲酸/乙酸铵溶液-0.1%(v/v)甲酸/甲醇溶液为流动相,以Accucore C18为分析柱进行梯度洗脱;在电喷雾电离(ESI)正离子模式下测定;扫描方式为连续反应监测(CRM)。在考察的质量浓度范围内,7种乌头类生物碱的标准曲线符合二阶方程(权重因子1/x),相关系数为0.9991~0.9999;在全血和尿液中的方法检出限为0.02~0.60 ng/mL,在肝组织中的方法检出限为0.02~0.40 ng/g;加标回收率为91.1%~104.7%,日内精密度和日间精密度分别为0.2%~10.7%、1.0%~13.7%(n=6)。该方法简单准确,灵敏度高,能够满足生物样品中7种乌头类生物碱的快速分析。

关 键 词:连续反应监测  生物样品  乌头类生物碱  液相色谱-线性离子阱多级质谱法  在线固相萃取  
收稿时间:2015-10-29

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
ZHU Dingji,LU Minping,HUANG Kejian,ZHOU Zhe,LIN Cuiwu,YANG Ning,LIU Xiaofeng,QIAO Wentao,LI Lu,HUANG Xiaoqing.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[J].Chinese Journal of Chromatography,2016,34(3):249-257.
Authors:ZHU Dingji  LU Minping  HUANG Kejian  ZHOU Zhe  LIN Cuiwu  YANG Ning  LIU Xiaofeng  QIAO Wentao  LI Lu  HUANG Xiaoqing
Institution:1. Guangxi Zhuang Autonomous Region Academy for the Prevention and Treatment of Occupational Diseases, Nanning 530021, China; 2. School of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China; 3. Evidence Identification Center, Guangxi Zhuang Autonomous Region Public Security Department, Nanning 530012, China; 4. Thermo Fisher Scientific (China) Co., Ltd., Shanghai 201206, China
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 MSn fragments. The samples were treated with acetonitrile for protein precipitation, followed by dilution and centrifugation. The resulting solution was injected 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 0.9991 to 0.9999. 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 analytes, 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 aconitum alkaloids in biological samples.
Keywords:aconitum alkaloids  biological samples  consecutive reaction monitoring (CRM)  liquid chromatography-linear ion trap multistage mass spectrometry (LC-LIT/MSn)  on-line solid phase extraction (on-line SPE)  
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