药酒中乌头碱、次乌头碱、新乌头碱的LC／MS／MS分析  

Fast detection of aconitine,hypaconitine and mesaconitine in medicinal liquor by LC/MS/MS

作　　者：魏晓晓[1] 马博凯[1] 黄雯雯[1] 胡铁靖 刘伟丽[1] Wei Xiaoxiao;Ma Bokai;Huang Wenwen;Hu Tiejing;Liu Weili(Beijing Centre for Physical ＆ Chemical Analysis,Beijing Key Laboratory of Organic Materials Testing Technology ＆ Quality Evaluation,Beijing 100094,China)

机构地区：[1]北京市理化分析测试中心,有机材料检测技术与质量评价北京市重点实验室,北京100094

出　　处：《中国法医学杂志》2018年第3期294-296,共3页Chinese Journal of Forensic Medicine

摘　　要：目的应用高效液相色谱-质谱联用法对涉案药酒中有毒成分乌头碱、次乌头碱、新乌头碱快速定量分析。方法样品过膜后用乙腈稀释500倍,使用Waters ACQUITY UPLC BEN C18(100 mm×2.1 mm,1.7μm)色谱柱,以乙腈-10 mmol/L碳酸氢铵溶液(pH=10)为流动相梯度洗脱,多反应监测模式下测定涉案药酒中乌头生物碱的含量。设定方法下乌头碱、次乌头碱、新乌头碱的保留时间分别为5.10 min、5.64 min、4.58 min,用于定量分析的离子对(m/z)分别为646.6-586.6、616.6-556.6、632.7-572.6。在1~200 ng/mL内,乌头碱线性回归方程为Y=343.8X+38901(R2=0.9995);在100~1000 ng/mL内,次乌头碱线性回归方程为Y=3.817X-357.579(R2=0.9991);在0.5~10 ng/mL内,新乌头碱线性回归方程为Y=719.562X+128.748(R^2=0.9995)。用此方法检测出涉案药酒中乌头碱、次乌头碱、新乌头碱含量分别为71.85,415.86,1.49μg/mL。结论建立的高效液相色谱-质谱法可用于药酒中乌头碱、次乌头碱、新乌头碱的快速测定。Objective To develop a LC-MS/MS method for detection of aconitine, hypaconitine and mesaconitine in medicinal liquor. Methods The sample was diluted 500 times with acetonitrile after filtering. The analytical column used in this study was Waters ACQUITY UPLC BEN C18 （100mm × 2. lmm, 1.71xm） and the separation was performed by using acetonitrile containing 10 mmol/L ammonium bicarbonate as the mobile phases with gradient elution. Then the aconitum alkaloids were analyzed using LC/MS/MS in multiple reaction monitoring （MRM） mode. Results Under these certain chromatographic parameters the retention time of the aeonitine, hypaconitine and mesaeonitine were 5.10 min,5.64 min, 4. 58 min and the ion combinations of 646. 6 - 586. 6,616. 6 - 556. 6,632. 7 - 572. 6 were used for quantitative analysis, respectively. Within 1 ~ 200 ng/L, linear regression equation for aconitine was Y = 343. 8X ＋ 38901 （ R2 = 0. 9995 ）. Within 100 - 1000 ng/L, linear regression equation for hypaconitine was Y = 3. 817X - 357. 579 （ R2 = 0. 9991 ） . Within 0. 5 ~ 10ng/L, linear regression equation for mesaconine was Y = 719. 562X ＋ 128.748 （ R2 = 0. 9995 ）. The concentration of aconitine, hypaconitine and mesaconitine in medicinal liquor was 71.85,415.86 and 1.49 Ixg/mL, respectively. Conclusion This method developed was useful for analysis of aeonitine, hypaconitine and mesaconitine in medicinal liquor.

关 键 词：法医毒物分析 药酒 液相色谱-质谱联用 乌头碱 

分 类 号：DF795.3[医药卫生—法医学]