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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
其他题名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; 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
来源期刊色谱
ISSN1000-8713
出版年2016
卷号34期号:3页码:249-257
中文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/MS~n)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0.9991~0.9999;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。
英文摘要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/MS~n) 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 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 r~2 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 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.
中文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
英文关键词on-line solid phase extraction (on-line SPE) liquid chromatography-linear ion trap multistage mass spectrometry (LC-LIT/MS~n) consecutive reaction monitoring (CRM) aconitum alkaloids biological samples
语种中文
国家中国
收录类别CSCD
WOS类目CHEMISTRY ANALYTICAL
WOS研究方向Chemistry
CSCD记录号CSCD:5675170
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/234694
作者单位1.广西壮族自治区职业病防治研究院, 南宁, 广西 530021, 中国;
2.广西大学化学化工学院, 南宁, 广西 530004, 中国;
3.广西壮族自治区公安厅物证鉴定中心, 南宁, 广西 530012, 中国;
4.赛默飞世尔科技(中国)有限公司, 上海 201206, 中国
推荐引用方式
GB/T 7714
朱定姬,卢敏萍,黄克建,等. 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],2016,34(3):249-257.
APA 朱定姬.,卢敏萍.,黄克建.,周哲.,林翠梧.,...&黄晓青.(2016).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.色谱,34(3),249-257.
MLA 朱定姬,et al."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".色谱 34.3(2016):249-257.
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