超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定动物源性产品中氟吡草酮及其代谢物残留量  

Determination of Bicyclopyrone and Its Metabolite Residues in Animal-derived Products by Ultra-high Performance Liquid Chromatography-Quadrupole/Orbitrap High Resolution Mass Spectrometry

作　　者：陈高群 荣杰峰 乐有东 龚慧婷 张松艳 张志勇 佘紫文 CHEN Gaoqun;RONG Jiefeng;LE Youdong;GONG Huiting;ZHANG Songyan;ZHANG Zhiyong;SHE Ziwen(Quanzhou Customs Comprehensive Technology Service Center,Quanzhou 362000)

机构地区：[1]泉州海关综合技术服务中心,福建泉州362000

出　　处：《分析科学学报》2023年第3期302-308,共7页Journal of Analytical Science

基　　金：福建省农产品质量安全重点实验室开放课题(KFKT-2020-5)。

摘　　要：建立了超高效液相色谱-四极杆/静电轨道阱高分辨质谱法检测动物源性产品中氟吡草酮及其代谢物残留量的方法。样品经甲酸-乙腈溶液提取,分散固相萃取净化,以甲醇-0.2%甲酸水溶液为流动相进行梯度洗脱分离,采用高分辨质谱平行反应监测扫描模式,以正离子模式进行定性定量分析,基质匹配外标法定量。结果表明,氟吡草酮在0.002~0.2μg/L范围、其代谢物SYN503780和代谢物CSCD686480在0.1~10μg/L范围线性关系良好,相关系数均大于0.995。空白样品在低、中、高3个加标水平下的平均回收率为84.5%~107.9%,相对标准偏差(RSD,n=6)为3.5%~8.6%;方法定量限为0.01~0.5μg/kg。该方法可应用于动物源性产品中氟吡草酮及其代谢物的快速检测。A method for the determination of bicyclopyrone and its metabolite residues in animal-derived products by ultra-high performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry was developed.The samples were extracted with formic acid-acetonitrile solution,and purified by dispersive solid phase extraction.The chromatographic analysis was performed on a Waters Acquity UPLC HSS T3 column with 0.2%formic acid solution and methanol as mobile phase by gradient elution,high resolution mass spectrometry parallel reaction monitoring scanning mode was used for qualitative screening and quantitative analysis by positive ion acquisition and a matrix matching external standard method was used for quantification.The results showed that the calibration curves of bicyclopyrone and metabolites(SYN503780 and CSCD686480)were linear in the range of 0.002-0.2μg/L and 0.1-10μg/L,respectively,with correlation coefficients greater than 0.995.The average recoveries of blank samples at low,medium and high levels were 84.5%-107.9%,the relative standard deviations(n=6)were 3.5%-8.6%,and the limit of quantitation were 0.01-0.5μg/kg.The method could be used for rapid detection of bicyclopyrone and its metabolites in animal-derived products.

关 键 词：氟吡草酮 代谢物 动物源性产品 超高效液相色谱-四极杆/静电轨道阱高分辨质谱法 

分 类 号：O657.63[理学—分析化学]