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. doi: 10.3724/SP.J.1123.2015.10044 shu

Citation: 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. doi: 10.3724/SP.J.1123.2015.10044 shu

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

朱定姬 ^1, ,
卢敏萍 ^2, ,
黄克建 ^{3,
,} ,
周哲 ^4, ,
林翠梧 ^2, ,
杨宁 ^3, ,
刘晓锋 ^3, ,
乔文涛 ^3, ,
李璐 ^3, ,
黄晓青 ^3,

1.
1. 广西壮族自治区职业病防治研究院, 广西南宁 530021;
2.
2. 广西大学化学化工学院, 广西南宁 530004;
3.
3. 广西壮族自治区公安厅物证鉴定中心, 广西南宁 530012;
4.
4. 赛默飞世尔科技(中国)有限公司, 上海 201206

通讯作者: 黄克建

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:

English

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

1.
1. Guangxi Zhuang Autonomous Region Academy for the Prevention and Treatment of Occupational Diseases, Nanning 530021, China;
2.
2. School of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China;
3.
3. Evidence Identification Center, Guangxi Zhuang Autonomous Region Public Security Department, Nanning 530012, China;
4.
4. Thermo Fisher Scientific (China) Co., Ltd., Shanghai 201206, China

Corresponding author: 黄克建

Received Date: 29 October 2015

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.

Key words:

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

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

通讯作者: 黄克建

English

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

Corresponding author: 黄克建

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

通讯作者: 黄克建

English

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

Corresponding author: 黄克建

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

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