›› 2013 ›› Issue (6): 50-53.
• Forensic System • Previous Articles Next Articles
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王毅1,刘子秋1,王炯2,黄勇王爱民4
通讯作者:
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
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
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
CLC Number:
R991
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.
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.
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