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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)
机构地区:[1]广检检测技术(上海)有限公司,上海201616 [2]广州检验检测认证集团有限公司国家加工食品质量监督检验中心(广东),广东广州511447
出 处:《中国酿造》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)。
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?>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.
关 键 词:QUECHERS 气相色谱-串联质谱法 蔬菜 琥珀酸脱氢酶抑制剂类
分 类 号:TS202.3[轻工技术与工程—食品科学]
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