葡萄酒中16种真菌毒素的同位素稀释-超高效液相色谱-串联质谱同时测定法  

Simultaneous determination of 16 kinds of mycotoxins in wine by isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry

作　　者：杨雪丽[1] 王猛[1] 李菁[1] 李方[1] YANG Xue-li;WANG Meng;LI Jing;LI Fang(Health Monitoring and Inspection Center,Xinjiang Uygur Autonomous Region Center for Disease Prevention and Control,Urumqi Xinjiang,830001,China)

机构地区：[1]新疆维吾尔自治区疾病预防控制中心卫生监测检验中心,新疆乌鲁木齐830001

出　　处：《职业与健康》2023年第11期1447-1454,共8页Occupation and Health

基　　金：新疆维吾尔自治区自然科学基金(2020D01C083)。

摘　　要：目的 建立稳定同位素内标超高效液相色谱-串联质谱联用法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)检测葡萄酒中16种真菌毒素的分析方法。方法 葡萄酒样品经乙腈提取后盐析,上清液用纯水1∶1稀释后过0.22μm聚四氟乙烯针式滤膜,加入稳定同位素内标降低基质效应。采用ACQUITY UPLCBETH C18色谱柱(100 mm×2.1 mm,1.7μm)分离,多反应监测模式(multiple reaction monitoring,MRM)下电喷雾离子源正、负离子模式,内标法定量。结果 16种真菌毒素在一定浓度范围内具有良好的线性关系,相关系数(r)均>0.999,方法检出限(limit of detection,LOD)在0.1~50.0μg/kg之间,方法定量限(limit of quantification,LOQ)为0.3~165.0μg/kg。在3个浓度的加标水平下,平均回收率为在62.7%~117.5%之间,相对标准偏差为2.0%~9.5%(n=6)。结论 该方法操作简单、高效、成本低,具有较好的准确度和精密度,可用于大批量葡萄酒中16种真菌毒素的快速、准确定量检测。Objective To establish a method for the simultaneous determination of 16 kinds of mycotoxins in wine by isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The wine samples were extracted by acetonitrile,the extract was salted out and dehydration.The supernatant diluted with water 1:1 and then filtrated with 0.22μm polytetrafluoroethylene millipore filter,the matrix effects were efficiently reduced with the stable isotope.The target substances were separated on ACQUITY UPLCBETH C18(100 mmx2.1 mm,1.7μm).The multiple reaction monitoring(MRM)mode was used for detection in electrospray ionization with positive and negative ion modes,and quantified by internal standard method.Results There was a good linearity for 16 kinds of mycotoxins within a certain concentration range,the correlation coefficients(r)were greater than 0.999,the limits of detection(LOD)and limit of quantification(LOQ)were 0.1-50.0μg/kg and 0.3-165.0μg/kg,respetively.The average recoveries were 62.7%-117.5%at three different levels,and the relative standard deviations were 2.0%-9.5%(n=6).Conclusion The method is simple,efficient,low-consumption,and has good accuracy and precision,which is uitable for the rapid and accurate quantitative detection of 16 mycotoxins in large quantities of wine.

关 键 词：真菌毒素 同位素稀释 葡萄酒 超高效液相色谱-串联质谱 

分 类 号：R115[医药卫生—公共卫生与预防医学]