超高效液相色谱—串联质谱法测定泡制酒中7种乌头类生物碱

Determination of 7 aconitum alkaloids in soaking wine with UPLC-MS-MS

目的建立泡制酒中乌头碱、次乌头碱、新乌头碱、草乌甲素、滇乌头碱、雪上一枝蒿甲素和雪上一枝蒿乙素的超高效液相色谱—串联质谱(UPLC-MS-MS)的测定方法。方法2021年5月,采用超高效液相色谱—串联质谱法对送检的一份泡制酒样本检测,经稀释、涡旋、离心及混匀等前处理后经0.22μm滤膜过滤,直接进样检测分析。色谱柱为ACQUITY UPLC BEH C181.7μm 2.1×100 mm Column,流动相为0.1%甲酸水溶液—乙腈,10 min梯度洗脱,质谱分析采用电喷雾离子源(正离子扫描ESI+)模式和多反应监测(MRM)模式。结果本次试验采用0.1%甲酸水溶液—乙腈流动相及梯度洗脱程序,所有目标物在8 min内被全部洗脱,且线性良好分离度高;7种乌头类生物碱的线性范围在25~500μg/L,相关系数均大于0.999,方法检出限0.06~7.78μg/L,定量下限0.20~26.0μg/L,加标回收率范围82.6%~118.9%,相对标准偏差范围在0.6%~5.6%。结论该方法操作简便、准确度好,可快速检测样本中7种乌头类生物碱,满足突发公共卫生事件中快速鉴定目标物的需要。

Objective To establish the method to detect the aconitine,hypaconitine,neoaconitine,aconitine,aconitine,artemisinin A and B in soaking wine with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MSMS).Methods In May 2021,a sample of soaking wine was detected with UPLC-MS/MS method by pretreatment of dilution,vortex,centrifugation and mixing,then injected the samples for determination after filtered with 0.22μm filter membrane.The chromatographic column was the ACQUITY UPLC BEH C181.7μm 2.1×100 mm column.The mobile phase was 0.1%formic acid aqueous solution acetonitrile,10 minutes gradient elution.The electrospray ion source(positive ion scanning)mode and multi reaction monitoring(MRM)mode were adopted for mass spectrometry analysis.Results The mobile phase was 0.1%formic acid aqueous solution acetonitrile,and the gradient elution procedure was adopted.All the target substances were eluted within 8 minutes,with good antecedency and high separation degree.The linear range of 7aconitum alkaloids was 25-500μg/L,the correlation coefficients were all greater than 0.999.In this method,the detection limit was 0.06-7.78μg/L,the lower limit of quantification was 0.20-26.0μg/L,the range of adding standard recovery rate was from 82.6%to 118.9%,and the relative standard deviation ranged from 0.6%to 5.6%.Conclusions This method is easy handle with high accuracy.It can quickly detect 7 aconitum alkaloids in soaking wine,and meets the requirement of rapid identification of target substances in the public health emergencies.