| 高效液相色谱-质谱联用法同时测定全血中雪上一枝蒿中6种生物碱 |
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| 引用本文： | 赵万江,杨福成,裴雯,冷晓晓,施丝,张茂林. 高效液相色谱-质谱联用法同时测定全血中雪上一枝蒿中6种生物碱[J]. 职业卫生与应急救援, 2021, 39(4): 459-462. DOI: 10.16369/j.oher.issn.1007-1326.2021.04.021 |
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| 作者姓名： | 赵万江 杨福成 裴雯 冷晓晓 施丝 张茂林 |
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| 作者单位： | 重庆市职业病防治院/职业病防治与中毒救治重庆市重点实验室, 重庆 400060 |
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| 基金项目： | 重庆市科卫联合医学科研项目2018MSXM062 |
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| 摘 要： | 目的 采用高效液相色谱-质谱联用法(HPLC-MS/MS)建立一种全血中同时测定雪上一枝蒿中6种生物碱(乌头碱、次乌头碱、新乌头碱、滇乌头碱、雪上一枝蒿甲素及雪上一枝蒿乙素)的快速、灵敏的检测方法.方法 采用Waters C18色谱柱,以甲醇-甲酸(两者体积分数为0.1％)水溶液为流动相,梯度洗脱,流速0.2 mL/m...
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| 关 键 词： | 高效液相色谱-质谱联用法 雪上一枝蒿 乌头碱 同时检测 |
| 收稿时间： | 2020-11-30 |
Simultaneous quantification of six alkaloids in aconitum brachypodum in whole blood by HPLC-MS/MS |
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| Abstract: | Objective To develop a HPLC-MS/MS method for simultaneous quantification of six alkaloids, namely aconitine, hypaconitine, mesaconitine, yunaconitine, bullatine A and bullatine B, in aconitum brachypodum in blood. Methods The gradients were eluted with methanol-water with 0.1% formic acid as mobile phase and separated on Waters C18 column. The flow rate was 0.2 mL/min. Protein precipitation with acetonitrile was used in sample preparation. Electrospray ionization, multiple reaction monitoring scan mode were used for mass spectrometry detection. Results The linear ranges were 0.5-100 ng/mL for six alkaloids. The limits of aconitine, hypaconitine, mesaconitine, yunaconitine, bullatine A and bullatine B were found to be 0.50, 0.26, 0.56, 0.03, 0.30 and 0.20 ng/mL, respectively. At three spiked concentrations, the average extraction recoveries ranged from 82.1%-90.3%, accuracy ranged from 98.9%-105.8%. The intra-day and inter-day RSDs were less than 7%. Conclusions The method provides a sensitive, accurate, precise and reliable analytical procedure for clinical and toxicological monitoring of six alkaloids in aconitum brachypodum in whole blood. |
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