UPLC-MS/MS法测定人血中雪上一枝蒿甲素

›› 2013 ›› Issue (6): 50-53.

UPLC-MS/MS法测定人血中雪上一枝蒿甲素

王毅¹,刘子秋¹,王炯²,黄勇王爱民⁴

收稿日期:2013-08-09 修回日期:2013-08-26 出版日期:2013-11-15 发布日期:2013-11-28
通讯作者: 王毅
基金资助:
贵州省优秀科技教育人才省长专项资金项目;贵阳市科技计划项目

Determination of Bullatine A in Human Blood by UPLC-MS/MS

Received:2013-08-09 Revised:2013-08-26 Published:2013-11-15 Online:2013-11-28

摘要/Abstract

摘要： 目的建立超高效液相色谱-串联质谱（UPLC-MS/MS）法测定人血中雪上一枝蒿甲素含量的方法。方法样品经乙酸乙酯提取后，C18柱分离，以0.1%甲酸乙腈-0.1%甲酸水为流动相梯度洗脱，正离子-多反应离子监测模式（ESI+-MRM）测定雪上一枝蒿甲素，定性定量离子对分别为344.3/58.0、344.3/91.0。结果雪上一枝蒿甲素在3.5～850μg/L-1范围内与峰面积呈现良好的线性关系（r=0.9968），检测限为0.1μg/L-1，日内、日间精密度均＜10％，低、中、高三个浓度下准确度（n=5）为97.2％～115.2％，回收率（n=5）为86.6％～89.4％。结论该方法操作简便，结果准确，可作为测定人血中雪上一枝蒿甲素含量的方法。

关键词: font-size: 10.5pt, mso-bidi-font-size: 10.0pt, mso-fareast-font-family: 宋体, mso-font-kerning: 1.0pt, mso-ansi-language: EN-US, mso-fareast-language: ZH-CN, mso-bidi-language: AR-SA" lang="EN-US">UPLC-MS/MSfont-size: 10.5pt, mso-ascii-font-family: 'Times New Roman', mso-hansi-font-family: 'Times New Roman', mso-bidi-font-size: 10.0pt, mso-font-kerning: 1.0pt, mso-bidi-font-family: 'Times New Roman', mso-ansi-language: EN-US, mso-fareast-language: ZH-CN, mso-bidi-language: AR-SA">；人血；雪上一枝蒿甲素

Abstract: Objective To determine bullatine A in human blood by UPLC-MS/MS. Methods The sample was extracted with acetic ether and separated on a C18 column using, 0.1% formic acid and acetonitrile as mobile phase． The positive electrospray ionization source was used. The ion pairs for the anaylsis of bullatine A were 344.3/58.0 and 344.3/91.0 in the multiple reaction monitoring mode. Results Linear relationship between peak area and concentration of bullatine A was obtained in the range of 3.5-850 μg/L-1 （r=0.9968）. The limit of detection for the analyte was 0.1μg/L-1. Relative standard deviations （RSD）（n=6） for the intra-day and inter-day precisions were lower than 10%. At three spiked concentrations, accuracy （n=5） ranged from 97.2% to 115.2%, and recovery ranged from 86.6% to 89.4%． Matrix effect was not obvious. Conclusion The established method is simple, sensitive, and accurate. It can be used for the determination of bullatine A in human blood．

Key words:

, ultra-performance liquid chromatography tandem mass spectrometry；human blood；bullatine A

中图分类号:

R991

王毅, 刘子秋, 王炯, 黄勇, 王爱民. UPLC-MS/MS法测定人血中雪上一枝蒿甲素[J]. , 2013(6): 50-53.

WANG Yi, LIU Zi-Qiu, WANG Jiong, HUANG Yong, WANG Ai-Min. Determination of Bullatine A in Human Blood by UPLC-MS/MS[J]. , 2013(6): 50-53.

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