QuEChERS-同位素内标-高效液相色谱-串联质谱法测定果蔬中灭蝇胺残留

Determination of Cyromazine in the Fruits and Vegetables by QuEChERS-Internal Standard-High Performance Liquid Chromatography-Tandem Mass Spectrometry

目的:建立高效液相色谱-串联质谱法(HPLC-MS/MS)测定果蔬中灭蝇胺的分析方法。方法:样品经氨化乙腈(含1%氨水,v/v)提取后,通过优化的QuEChERS(900 mg无水硫酸镁、300 mg C_(18)、300 mg PSA)方法获得净化液,净化液最后离心后直接过膜上机检测。HPLC-MS/MS方法以甲酸-乙酸铵水(含0.1%甲酸,v/v;5 mmol/L乙酸铵)和乙腈为流动相,流速0.3 mL/min,采用HILIC色谱柱、电喷雾正离子模式(ESI^(+))、多反应监测(MRM)检测及基质匹配内标法定量。结果:在9种基质(菠菜、番茄、豇豆、葡萄、莲藕、生姜、火龙果、芒果、苹果)中,灭蝇胺在0.5~20 ng/mL质量浓度与其对应的峰面积之间线性关系良好,R^(2)均大于0.994,在0.005、0.01 mg/kg和0.05 mg/kg 3个添加水平下,灭蝇胺的平均回收率在89%~107%之间,相对标准偏差在0.8%~5.4%之间。结论:QuEChERS-同位素内标-高效液相色谱-串联质谱法的准确度、精密度和灵敏度均符合灭蝇胺残留检测的要求。

Objective:To establish an analytical method for the determination of cyromazine in fruits and vegetables by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods:The sample was extracted with ammoniated acetonitrile(containing 1%ammonia water,v/v),and purified by the optimized QuEChERS(900 mg anhydrous magnesium sulfate,300 mg C_(18),300 mg PSA)method,and the purified solution was centrifuged and filtrated before detection.The HPLC-MS/MS method used formic acid-ammonium acetate water(containing 0.1%formic acid,v/v;5 mmol/L ammonium acetate)and acetonitrile as mobile phases.The flow rate was 0.3 mL/min gradient elution.HILIC chromatographic column,electrospray positive ionization(ESI+),multiple reaction monitoring(MRM)and matrix-matched internal standard method were used for quantification.Results:In 9 substrates(spinach,tomato,cowpea,grape,lotus root,ginger,pitaya,mango,apple),there was a good linear relationship between the mass concentration of cyromazine and its corresponding peak area at 0.5~20 ng/mL.R^(2) was all greater than 0.994.At the 3 levels of 0.005,0.01,0.05 mg/kg,the average recovery of cyromazine was between 89%~107%,and the relative standard deviation was between 0.8%~5.4%.Conclusion:The accuracy,precision and sensitivity of the method meet the requirements of cyromuzine residue detection.