不同蔬菜中氟虫腈及其代谢物检测方法的确定与比较  

Determination and Comparison of Detection Methods of Fipronil and Its Metabolites in Different Vegetables

作　　者：周玉春 滕玉娇 王少龙 刘慧 李其亮[1] 谢文东 孙娅娜 黄华[1] ZHOU Yuchun;TENG Yujiao;WANG Shaolong;LIU Hui;LI Qiliang;XIE Wendong;SUN Yana;HUNANG Hua(Beijing Products Quality Supervision and Inspection Institute,Beijing 101300,China;College of Food Science and Nutritional Engineering,China Agricultural University,Beijing 100083,China)

机构地区：[1]北京市产品质量监督检验院,北京101300 [2]中国农业大学食品科学与营养工程学院,北京100083

出　　处：《现代食品》2021年第6期194-198,共5页Modern Food

摘　　要：本研究建立了气相色谱-质谱联用仪测定氟虫腈及其3种代谢物的方法,并对比了不同固相萃取柱对氟虫腈及其代谢物回收率的影响。结果表明,仪器方法选用DB-5MS毛细管柱(30 m×0.25 mm×0.25μm),气相色谱-质谱联用仪带负离子化学源(NCI),最终确定氟甲腈选择监测离子为(m/z)352,353,354;氟虫腈砜选择监测离子为(m/z)383,347,416,385;氟虫腈亚砜选择监测离子为(m/z)384,385,386;氟虫腈选择监测离子为(m/z)366,333,368,400。使用丙基乙二胺键合硅胶固相萃取柱的回收率比C18反相固相萃取柱、氨基固相萃取柱和石墨化碳黑固相萃取柱组合柱回收率高,且操作更加简单、高效。In this study,a method for the determination of fipronil and its three metabolites by gas chromatographymass spectrometry was established,and the effects of different solid phase extraction columns on the recovery of fipronil and its metabolites were compared.The results showed that the instrument method used DB-5 MS capillary column(30 m×0.25 mm×0.25μm),gas chromatography-mass spectrometer with negative chemical ionization(NCI),and finally determined that the selected monitoring ion of fipronil-desulfinyl was(m/z)352,353,354;fipronil sulfone selective monitoring ion is(m/z)383,347,416,385;fipronil-sulfide selective monitoring ion is(m/z)384,385,386;fipronil selective monitoring ion is(m/z)366,333,368,400.The recovery rate of using propyl ethylenediamine bonded silica gel solid phase extraction column is higher than that of C18 reversed phase solid phase extraction column,amino solid phase extraction column and graphitized carbon black solid phase extraction column combined column,and the operation is simpler and efficient.

关 键 词：氟虫腈 代谢物 气相色谱 负离子化学源 质谱 

分 类 号：TS207.3[轻工技术与工程—食品科学]