固相萃取/超高效液相色谱-串联质谱法测定稻渔水体中氟虫腈及其代谢物  

Determination of Fipronil and Its Metabolites in Rice Fishing Water Samples by SPE/UPLC-MS/MS

作　　者：马丽莎[1] 郑光明[1] 尹怡[1] 谢文平[1] 单奇[1] 林嘉薇 李丽春[1] 刘书贵[1] 赵城[1] 戴晓欣[1] 魏琳婷 MA Li-sha;ZHENG Guang-ming;YIN Yi;XIE Wen-ping;SHAN Qi;LIN Jia-wei;LI Li-chun;LIU Shu-gui;ZHAO Cheng;DAI Xiao-xin;WEI Lin-ting(Guangdong Provincial Key Laboratory of Aquatic Animal Immunology and Sustainable Aquaculture,Key Laboratory of Prevention and Control for Aquatic Invasive Alien Species,Ministry of Agriculture and Rural Affairs,Pearl River Fisheries Research Institute,Chinese Academy of Fishery Sciences,Guangzhou 510380,China)

机构地区：[1]中国水产科学研究院珠江水产研究所,农业农村部外来入侵水生生物防控重点实验室,广东省水产动物免疫与绿色养殖重点实验室,广东广州510380

出　　处：《分析测试学报》2022年第11期1678-1683,共6页Journal of Instrumental Analysis

基　　金：国家水产品质量安全风险评估专项(GJFP201800902);中国-东盟海上合作基金项目(CAMC-2018F)。

摘　　要：利用固相萃取(SPE)/超高效液相色谱-串联质谱(UPLC-MS/MS)建立了稻渔水体中氟虫腈及其代谢物(氟甲腈、氟虫腈砜和氟虫腈亚砜)的分析方法。根据目标物的化学性质及稻渔水样的基质情况,筛选出适用于稻渔水样预处理的滤膜及稻渔水体中目标物的萃取方法,并对固相萃取条件、氮吹温度等参数进行优化。稻渔水样经玻璃纤维滤纸过滤后,由Supelco ENVI-18固相萃取柱富集、净化,采用SB-C_(18)柱(2.1 mm×100 mm,1.8μm)进行分离,在电喷雾电离源负离子模式下进行检测,外标法定量。结果显示:目标物在0.5~100 ng/mL范围内线性关系良好,相关系数(r^(2))大于0.998,检出限为0.5 ng/L,定量下限为1.5 ng/L;在2、5、50 ng/L加标水平下的回收率为81.6%~105%,相对标准偏差为3.5%~7.0%。该方法操作简便、灵敏、高效、性价比高,可用于稻渔水体中氟虫腈及其代谢物的同时测定。A solid-phase extraction(SPE)/ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed for the determination of residues of fipronil(FIP)and its metabolites(FIP_(S)),i.e.fipronil desulfinyl,fipronil sulfone and fipronil sulfide in rice fishing water.According to the complicated properties of the testing chemicals and the impurities of rice fishing water samples,a new type of filter membrane was selected for the pretreatment of water sam⁃ples,and the following extraction method was successfully exploited after a series of preliminary experiments.Furthermore,the SPE conditions and nitrogen blowing temperatures were optimized to ensure the high efficiency of extraction and high purification quality of extraction.In brief,rice fish⁃ing water samples were firstly filtered by using glass fiber filter paper,then enriched and purified with Supelco ENVI-18 solid-phase extraction column,and finally eluted with acetonitrile.The tar⁃get compounds were separated on a SB-C_(18) column(2.1 mm×100 mm,1.8μm),and subsequent⁃ly determined using an electrospray ionization source in the negative ion multiple reaction monitoring(MRM)mode.The calibration curves for target compounds were linear in the range of 0.5-100 ng/mL with correlation coefficients(r^(2))more than 0.998.The limits of detection(LODs)and quantitation(LOQs)were 0.5 ng/L and 1.5 ng/L,respectively.The average recoveries for target compounds ranged from 81.6%to 105%,with relative standard deviations(RSDs)of 3.5%-7.0%.The pro⁃posed method was applied to the determination of FIP and FIPS in thirteen authentic water samples col⁃lected from the rice fishing areas,of which one was found containing fipronil and fipronil sulfone.The proposed method is simple,sensitive,cost-effective and efficient,and could provide technical support for the environmental monitoring and risk assessment of FIP and FIPS in rice fishing systems and their food products.

关 键 词：超高效液相色谱-串联质谱 固相萃取 稻渔水体 氟虫腈及其代谢物 

分 类 号：O657.31[理学—分析化学] X832[理学—化学]