稳定同位素稀释超高效液相色谱-串联质谱法测定饲料中氟虫腈及其代谢物

引用本文: 周鹏, 黄芊, 欧阳立群, 王征, 孟鹏, 戴明, 王瑛. 稳定同位素稀释超高效液相色谱-串联质谱法测定饲料中氟虫腈及其代谢物[J]. 色谱, 2018, 36(7): 629-633. doi: 10.3724/SP.J.1123.2018.01049 shu

Citation: ZHOU Peng, HUANG Qian, OUYANG Liqun, WANG Zheng, MENG Peng, DAI Ming, WANG Ying. Determination of fipronil and its metabolites in feeds by stable isotope dilution ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(7): 629-633. doi: 10.3724/SP.J.1123.2018.01049 shu

稳定同位素稀释超高效液相色谱-串联质谱法测定饲料中氟虫腈及其代谢物

周鹏 ^1,2, ,
黄芊 ^2, ,
欧阳立群 ^2, ,
王征 ^2, ,
孟鹏 ^2, ,
戴明 ^2, ,
王瑛 ^1,

1.
南京理工大学化工学院, 江苏南京 210094;
2.
国家加工食品质量监督检验中心(福州), 福建福州 350002

摘要: 建立了超高效液相色谱-串联质谱测定饲料中氟虫腈及其代谢物氟甲腈、氟虫腈硫醚和氟虫腈砜的方法。样品经纯水和乙腈超声提取后加入氯化钠盐析，采用QuEChERS技术净化，以Waters HSS T3 C₁₈色谱柱分离，甲醇和纯水为流动相进行梯度洗脱，在多反应监测、负离子模式下进行检测，内标法定量。氟虫腈及其代谢物在各自的范围内呈良好的线性关系，相关系数均大于0.9998；氟虫腈及其代谢物的检出限和定量限分别为0.05 μg/kg和0.2 μg/kg，加标回收率为92.3%~105.4%，相对标准偏差为0.9%~2.3%（n=5）。该法样品前处理过程简单，净化效果好，灵敏度高，适用于各种饲料中氟虫腈及其代谢物含量的测定。

关键词:

English

Determination of fipronil and its metabolites in feeds by stable isotope dilution ultra high performance liquid chromatography-tandem mass spectrometry

1.
School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China;
2.
National Center for Quality Supervision Inspection of Processed Foods(Fuzhou), Fuzhou 350002, China
Received Date: 30 January 2018

Abstract: A method based on ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was established for the determination of fipronil and its metabolites in feeds. Sodium chloride was added to the samples after the ultrasonic extraction of pure water and acetonitrile, and then cleaned up by the QuEChERS method. The target analytes were separated on a Waters HSS T3 C₁₈ column using methanol and water as mobile phases with gradient elution, and detected by a MS/MS system under negative electro-spry ionization (ESI^-) and the multiple reaction monitoring (MRM) mode. The limits of detection (LODs) were 0.05 μg/kg, and the limits of quantification (LOQs) were 0.2 μg/kg. The linear correlation coefficients were more than 0.9998. The average recoveries ranged from 92.3% to 105.4% with RSDs no more than 2.3%. This method is suitable for the identification of fipronil and its metabolites in feeds because of its simplicity and high sensitivity.

Key words:

ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)
/ QuEChERS
/ isotope dilution
/ fipronil and its metabolites
/ feeds

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沈阳化工大学材料科学与工程学院沈阳 110142

稳定同位素稀释超高效液相色谱-串联质谱法测定饲料中氟虫腈及其代谢物

English

Determination of fipronil and its metabolites in feeds by stable isotope dilution ultra high performance liquid chromatography-tandem mass spectrometry

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

稳定同位素稀释超高效液相色谱-串联质谱法测定饲料中氟虫腈及其代谢物

English

Determination of fipronil and its metabolites in feeds by stable isotope dilution ultra high performance liquid chromatography-tandem mass spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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通讯作者: 陈斌, bchen63@163.com

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