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  

Rapid determination of fipronil and its metabolites in egg and chicken by QuEChERS-solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

作　　者：夏义平[1] 尹啸冰 林肖惠[1] 田阳光 XIA Yi-ping;YIN Xiao-bing;LIN Xiao-hui;TIAN Yang-guang(Tianjin Center for Disease Control and Prevention,Tianjin 300011,China;Tianjin Hexi District Center for Disease Control and Prevention,Tianjin 300201,China)

机构地区：[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

出　　处：《中国食品卫生杂志》2018年第4期395-400,共6页Chinese Journal of Food Hygiene

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,2.0μm)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0.5～20.0μg/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、0.05μg/kg,在添加水平为0.5、2.0、10.0μg/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。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）. Acetonitrilewater 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 offipronil 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% to105. 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.

关 键 词：QUECHERS 鸡蛋 鸡肉 氟虫腈 高效液相色谱-串联质谱 兽药残留 检测方法 

分 类 号：R155[医药卫生—营养与食品卫生学]