摘要
建立了气相色谱-串联质谱法(GC-MS/MS)同时测定蔬菜中9种琥珀酸脱氢酶抑制剂类(SDHIs)化合物。样品以10 mL乙腈提取后,盐析分层,上清液使用30 mg N-丙基乙二胺(PSA)和30 mg十八烷基硅烷键合硅胶(C18)固相萃取剂进行净化,氮气浓缩后使用乙酸乙酯复溶。9种琥珀酸脱氢酶抑制剂类化合物通过气相色谱分离,电子轰击源离子化,多反应监测(MRM)模式采集离子对。结果表明,9种SDHIs均在各自的浓度范围内呈现良好的线性关系,相关系数R^(2)>0.994,方法检出限(LODs)为1.00~6.00μg/kg,定量限(LOQs)为3.00~20.0μg/kg。9种SDHIs的不同水平加标实验结果为回收率在80.4%~98.2%,精密度实验结果相对标准偏差(RSDs)为3.0%~7.9%。该方法高效快速,操作简便,检测成本低,且回收率高、灵敏度高、重现性好,适用于日常蔬菜中9种SDHIs批量测定。
A gas chromatography-tandem mass spectrometry(GC-MS/MS)method was established for the simultaneous determination of 9 succinate dehydrogenase inhibitor(SDHIs)compounds in vegetables.Samples were extracted with 10 ml acetonitrile,then salted out to separate the layers.The supernatant was purified using 30 mg N-primary secondary amine(PSA)and 30 mg octadecylsilane chemically bonded silica(C18)solid phase extrac-tion agent,concentrated under nitrogen and dissolved with ethyl acetate.9 SDHIs were separated by gas chromatography and ionized by electron ion-ization(EI)source,while the ion pairs were collected by multiple reaction monitoring(MRM)mode.The results showed that 9 SDHIs showed good linear relationships within their respective concentration ranges.The correlation coefficient R^(2)>0.994,the limits of detection(LODs)of method ranged 1.00-6.00μg/kg,while the limits of quantification(LOQs)ofmethod ranged 3.00-20.0μg/kg.The results of different levels of spiked experiments for 9 SDHIs showed a good recovery rate of 80.4%-98.2%and the relative standard deviations(RSDs)were 3.0%-7.9%.The method was efficient,fast,easy to operate,with low detection cost,high recovery rate,high sensitivity,and good reproducibility,which was suitable for batch determination of 9SDHIs indailyvegetables.
作者
刘军
罗先勇
曹巧凤
李吉龙
张博
岑建斌
李姗
LIU Jun;LUO Xianyong;CAO Qiaofeng;LI Jilong;ZHANG Bo;CEN Jianbin;LI Shan(GTTC Testing Technology(Shanghai)Co.,Ltd.,Shanghai 201616,China;National Quality Testing Center for Processed Food(Guangdong),Guangzhou Inspection and Testing Certification Group Co.,Ltd.,Guangzhou 511447,China)
出处
《中国酿造》
北大核心
2025年第4期290-296,共7页
China Brewing
基金
广州市市场监督管理局科技项目(2021kj57)。
