超高效液相色谱-串联质谱法快速测定雷公藤中毒样品中4种毒性成分  

Rapid determination of four toxic components in Tripterygium Wilfordii poisoning samples by ultra high performance liquid chromatography-tandem mass spectrometry

作　　者：华正罡[1] 陈曦[1] 冯静[1] Hua ZhengGang;Chen Xi;Feng Jing(Liaoning Center for Disease Control and Prevention,Liaoning Provincial Key Laboratory of Air Haze and Human Health Monitoring,Shenyang 110005,China)

机构地区：[1]辽宁省疾病预防控制中心,辽宁省空气雾霾与人群健康监测重点实验室,沈阳110005

出　　处：《化学分析计量》2021年第10期18-22,共5页Chemical Analysis And Meterage

摘　　要：建立超高效液相色谱-串联质谱(UPLC-MS/MS)法快速测定雷公藤中毒样品中雷公藤次碱、雷公藤晋碱、雷公藤甲素、雷公藤内酯甲4种主要毒性成分的方法。以Waters ACQUITY UPLC BEH C18柱(100 mm×2.1 mm,1.7μm)为分离柱,柱温为40℃,样品室温度为4℃,流动相A为乙腈,流动相B为10 mmol甲酸铵-0.1%甲酸溶液,梯度洗脱,流量为0.3 mL/min,进样体积为10μL,多反应监测(MRM)模式检测。在优化的仪器工作条件下,雷公藤次碱、雷公藤晋碱、雷公藤甲素、雷公藤内酯甲在各自的质量浓度范围内与色谱峰面积线性关系良好,线性相关系数均不小于0.9980,检出限分别为0.24、0.26、0.28、1.25 mg/kg。阴性样品加标平均回收率为83.7%~95.3%,测定结果的相对标准偏差为2.66%~5.71%(n=6)。该方法适用于雷公藤中毒样品的快速检测。A method of determination of wilforine,wilforgine,triptolide and wilforlide a in tripterygium wilfordii poisoning samples by ultra high performance liquid chromatography-tandem mass spectrometry was established.The chromatographic separation was carried out using Waters ACQUITY UPLC BEH C18 column(100 mm×2.1 mm,1.7μm)with column temperature at 40℃,the sample chamber temperature was 4℃,the mobile phase A was acetonitrile,the mobile phase B was 10 mmol ammonium formate-0.1%formic acid solution,gradient elution,the flow rate was 0.3 mL/min and the injection volume was 10μL.Multiple response monitoring(MRM)mode was used for the determination.Under the optimized working conditions of the instrument,the mass concentration of wilforine,wilforgine,triptolide and wilforlide A had a good linear relationship with the chromatographic peak area in their respective range,the linear correlation coefficients were not less than 0.9980,and the detection limits were 0.24,0.26,0.28 and 1.25 mg/kg,respectively.The average recoveries of negative samples were 83.7%-95.3%,and the relative standard deviations of determination results were 2.66%-5.71%(n=6).The method is suitable for the rapid detection of Tripterygium wilfordii poisoning samples.

关 键 词：超高效液相色谱-串联质谱法 雷公藤 雷公藤次碱 雷公藤晋碱 雷公藤甲素 雷公藤内酯甲 

分 类 号：O657.7[理学—分析化学]