超高效液相色谱-串联质谱快速检测食品中苯基吡唑类化合物质残留的方法

Detection of Phenylpyrazole Residues in Food by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry

建立了一种QuEChERS前处理方法结合超高效液相色谱-串联质谱技术检测食品中乙虫腈、丁虫腈、吡草醚、氟甲腈、氟虫腈、氟虫腈砜、氟虫腈亚砜和氟虫腈-脱三氟甲基亚砜等8种苯基吡唑类化合物残留的分析方法。针对不同的食品基质,使用φ=1%醋酸乙腈和水作为提取溶剂,经盐析和QuEChERS净化直接测定。以甲醇-水为流动相梯度洗脱,ESI离子源正负离子模式同时进行多反应监测模式(MRM)扫描,使用基质匹配标准溶液定量分析。苯基吡唑类化合物峰型尖锐对称,分离效果较好,在1~800μg/L范围内线性良好,相关系数大于0.99。该方法在鸡蛋、禽肉、牛奶、枣、白菜、茶叶、大米基质中检出限为0.01~0.53μg/kg之间,定量限为0.04~1.75μg/kg,加标回收率范围为70.12%~119.87%,相对标准偏差(RSD)为1.01%~9.91%(n=6)。该方法高效准确、通用性强,可应用于不同食品基质中苯基吡唑类化合物同时检测分析。

A food analytical method that combines QuEChERS pretreatment assay with ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)was developed for the detection of eight phenylpyrazole residues in food;ethiprole,flufiprole,pyraflufen-ethyl,fipronil-desulfinyl,fipronil,fipronil-sulfone,fipronil-sulfide,and fipronil-detrifluoromethyl sulfoxide.Different food matrices were directly measured by salting-out and QuEChERS purification using 1%acetonitrile acetate and water as extraction solvents.Gradient elution was conducted using methanol and water as the mobile phase and scanning in the multiple reaction monitoring(MRM)mode was performed simultaneously in the positive and negative ion ESI modes.Matrix-matched standard solutions were used for quantitative analysis.The peak shape of phenylpyrazoles was sharp and symmetrical,showing good separation effects,good linearity within the 1~800μg/L range,and correlation coefficients greater than 0.99.The detection limit of this method for eggs,poultry meat,milk,dates,Chinese cabbage,tea,and rice matrices ranged between 0.01~0.53μg/kg,with the quantitation limit at 0.04~1.75μg/kg,the standard recovery rates at 70.12~119.87%,and the relative standard deviation(RSD)from 1.01~9.91%(n=6).The developed QuEChERS-UHPLC-MS/MS method can be considered effective,accurate,and versatile,and it can be successfully applied for the simultaneous detection and analysis of different phenylpyrazole residues in food.