QuEChERS-液相色谱串联质谱法测定鲤肝脏中氟虫腈及其代谢物残留
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马丽莎(1981-),助理研究员,研究方向为水产品质量安全与风险评,E-mail:malisha16@163.com

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国家水产品质量安全风险评估-稻渔综合种养水产品安全性评估(GJFP201800902);海南省热带海洋生物技术重点实验室开放基金项目(LTMB201904);中国-东盟海上合作基金(CAMC2018F)


Determination of Fipronil and Its Metabolites in Liver Tissue of Cyprinus carpio by QuEChERS Combined with Liquid Chromatography-Tandem Mass Spectrometry
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    摘要:

    以QuEChERS作为样品前处理方法,结合高效液相色谱串联质谱(HPLC-MS/MS)检测技术,建立了鲤(Cyprinus carpio)肝脏中氟虫腈(fipronil)及代谢物氟甲腈(fipronil desulfinyl)、氟虫腈亚砜(fipronil sulfide)和氟虫腈砜(fipronil sulfone)的检测方法。样品用0.1%甲酸乙腈提取,提取液经吸附剂中性氧化铝、乙二胺-N-丙基硅烷(PSA)结合石墨炭化黑粉(GCB)净化,以LC-MS/MS进行测定,基质匹配标准曲线外标法定量。结果表明,鲤肝脏中4种目标物的平均回收率在87.3%~109.2%之间,相对标准偏差在1.3%~12.0%之间,氟虫腈及其代谢物在0.4~100.0 ng/mL线性范围内,线性良好,线性相关系数(r2)均大于0.997,检出限为2.0 μg/kg,定量限为5.0 μg/kg。该方法简单、快速且灵敏,单个样品前处理仅需20 min,适用于鲤肝脏中氟虫腈药物代谢及残留消除规律研究。[中国渔业质量与标准,2021,11(2):18-24]

    Abstract:

    A determination method of fipronil and its metabolites (fipronil desulfinyl,fipronil sulfide and fipronil sulfone) in liver tissue of Cyprinus carpio was developed by quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction coupled with high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). Samples were extracted with 0.1% formic acid acetonitrile, and purified by neutral alumina, PSA and GCB. Then, fipronil and its metabolites were detected by using LC-MS/MS. The analytes were quantified with external standard using the matrix-matched standard calibration curve method. The results showed that the average spiked recoveries of fiproni and its metabolites in liver tissue of fish were 87.3%~109.2%with relative standard deviations(RSDs) of 1.3%~12.0%. Good linearities were obtained in the range of 0.4~100.0 ng/mL, and the correlation coefficients were greater than 0.997, the LODs were 2.0 μg/kg, and the LOQs were 5.0 μg/kg. The method was simple, rapid and sensitive. And the preparation for a single sample was within 20min. The developed method is suitable for studying the metabolism and residue elimination of fipronil in fish liver. [Chinese Fishery Quality and Standards,2021,11(2):18-24]

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马丽莎,单奇,谢文平,等. QuEChERS-液相色谱串联质谱法测定鲤肝脏中氟虫腈及其代谢物残留[J].中国渔业质量与标准,2021,11(2):18-24. MA Lisha, SHAN Qi, XIE Wenping, et al. Determination of Fipronil and Its Metabolites in Liver Tissue of Cyprinus carpio by QuEChERS Combined with Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Fishery Quality and Standards,2021,11(2):18-24.

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  • 在线发布日期: 2021-04-22