QuEChERS-固相萃取-高效液相色谱-串联质谱法快速测定鸡蛋和鸡肉中氟虫腈及其代谢产物
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(1.天津市疾病预防控制中心,天津 300011;2.天津市河西区疾病预防控制中心,天津 300201)

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夏义平 男 主管技师 研究方向为食品安全及应急检测 E-mail:XYP_76@163.com通信作者:┣┣(中)通信作者┫┫马永民 男 主任技师 研究方向为食品安全及应急检测 E-mail:13662055367@163.com

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Rapid determination of fipronil and its metabolites in egg and chicken by QuEChERS-solid phase extraction-high performance liquid chromatography-tandem mass spectrometry
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(1.Tianjin Center for Disease Control and Prevention, Tianjin 300011, China;2.Tianjin Hexi District Center for Disease Control and Prevention,Tianjin 300201,China)

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    摘要:

    目的 建立一种QuEChERS-固相萃取(SPE)-高效液相色谱-串联质谱快速测定鸡蛋和鸡肉中氟虫腈及其代谢产物残留的方法。方法 鸡蛋和鸡肉样品经水-乙腈涡旋提取、QuEChERS盐析,SPE净化后,以XR-ODS柱(50 mm×3.0 mm,2.0 μm)为分析柱,以乙腈-水为流动相进行梯度洗脱,以负离子喷雾模式电离, 多反应离子监测方式进行定性及定量检测。结果 在0.5~20.0 μg/L的线性范围内,氟虫腈及其代谢产物的回归方程均呈良好的线性关系,r>0.999 2。氟虫腈、氟虫腈亚砜、氟虫腈砜、氟甲腈的检出限分别为0.2、0.05、0.05、0.05 μg/kg,在添加水平为0.5、2.0、10.0 μg/kg时,平均回收率在84.1%~105.2%之间,相对标准偏差(RSD)在1.3%~6.1%之间。结论 该方法前处理简便快捷,灵敏度和准确度均较高,精密度较好,适用于鸡蛋和鸡肉中氟虫腈及其代谢产物残留的检测。

    Abstract:

    Objective To develop a method for determination of fipronil and its metabolites in egg and chicken by QuEChERS-solid phase extraction(SPE)-high performance liquid chromatography-tandem mass spectrometry. Methods Egg and chicken samples were extracted by water-acetonitrile, the organic phase were salted out by QuEChERS,then cleaned up by SPE, loaded on a shimadzu XR-ODS column (50 mm×3.0 mm, 2.0 μm). Acetonitrile-water was used as the mobile phase gradient elution with negative ion spray mode ionization and multi-reactive ion monitoring (MRM) method for qualitative and quantitative detection. Results The matrix-matched calibration curve of fipronil and its metabites showed a good linear within the concentration range from 0.5 to 20.0 μg/L(r>0.999 2), the average recovery of fipronil and its metabolites at the spiked levels of 0.5,2.0 and 10.0 μg/kg was from 84.1%to 105.2%,and the relative standard deviation (RSD) was between 1.3% and 6.1%.The detection limits of fipronil, fipronil sulfone, fipronil sulfide, fluoronitrile were 0.2,0.05,0.05,0.05 μg/kg, respectively. Conclusion The method is simple rapid, highly sensitive and accurate. It is suitable for the detection of fipronil and its metabolites in egg and chicken.

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夏义平,尹啸冰,林肖惠,田阳光. QuEChERS-固相萃取-高效液相色谱-串联质谱法快速测定鸡蛋和鸡肉中氟虫腈及其代谢产物[J].中国食品卫生杂志,2018,30(4):395-400.

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  • 收稿日期:2018-02-09
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  • 在线发布日期: 2018-08-16
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