高效液相色谱-串联质谱法测定果蔬中6种氨基甲酸酯农药残留  

Determination of six pesticide residues in fruits and vegetables by high performance liquid chromatography-tandem mass spectrometry

作　　者：靳克林[1] 苏永恒[2] 张洁[2] 赵俊君[1] 朱文刚[1] 谢莉[1] JIN Kelin;SU Yongheng;ZHANG Jie;ZHAO Junjun;ZHU Wengang;XIE Li(Puyang Center for Disease Control and Prevention,Puyang,Henan 457000,China;Henan Center for Disease Control and Prevention)

机构地区：[1]濮阳市疾病预防控制中心,河南濮阳457000 [2]河南省疾病预防控制中心

出　　处：《河南预防医学杂志》2022年第7期537-540,562,共5页Henan Journal of Preventive Medicine

摘　　要：目的 建立一种测定氨基甲酸酯农药残留的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。方法 采用分散固相萃取法(Qu EChERS)处理样品,样品粉碎后乙腈提取,涡旋超声离心后提取液经 PSA 和 C18 吸附剂净化。以 20mmoL 乙酸铵的水溶液(含 0.1%乙酸)和乙腈为流动相梯度洗脱,C18 柱(100 mm×2.1 mm,2.6 μm)色谱柱分离样品中的6 种氨基甲酸酯农药残留。质谱分析则采用电喷雾离子源(ESI)正离子扫描,在多反应监测(MRM)模式下测定,保留时间和质谱特征碎片离子丰度比定性,外标法定量。结果 6 种氨基甲酸酯农药残留在 5 min 内得到有效分离,在 10~500μg/L范围内呈良好线性关系(r≥0.993),检出限(LOD)为 0.002~0.015 mg/kg,定量限(LOQ)为 0.005~0.050 mg/kg。空白样本中加 50 μg/L 和 200 μg/L 两个浓度水平混合标准溶液,6 种氨基甲酸酯农药残留加标回收率范围为 82.4%~95.6%,相对标准偏差(RSD)为 3.2%~6.5%。结论 该方法前处理简单、快捷,线性关系良好,灵敏度及准确度高,回收率好,能够为果蔬中氨基甲酸酯农药残留多组检测提供新思路。Objective To establish a high-performance liquid chromatography-mass spectrometry (HPLC-MS/MS) method for the determination of carbamate pesticide residues in fruits and vegetables. Methods The samples were processed by QuEChERS method. The samples were crushed, and extracted with acetonitrile, and after centrifugation by vortex ultrasonic centrifuge,the extracted liquid was purified by PSA and C18. Six carbamate pesticide residues were separated on a C18 column (100 mm×2.1 mm,2.6 μm) by gradient elution with a water containing 20 mmoL ammonium acetate combined with 0.1% acetic acid-acetonitrile as mobile phase. The analyses were detected by positive ion ESI in MRM mode, and they were qualitatively determined by retention time and mass spectrum characteristic fragment ion abundance ratio, and quantitatively determined with external standard method. Results Six carbamate pesticide residues were separated within 5 minutes efficiently. The method had a broad linearity in the range between 10 μg/L-500 μg/L with the correlative coefficients r~2≥0.993. The LOD was 0.002-0.015 mg/kg.The LOQ was 0.005 -0.050 mg/kg. The recovery rate of six carbamate pesticide residues was in range of 82.4% -95.6% with spike levels of 50 μg/L and 200 μg/L on blank sample, and the RSD was within 3.2%-6.5%. Conclusion The method is simple and rapid, and has a ,good liner relationship, high sensitivity, high accurateness, and good recovery, which can provide a new idea for the determination of carbamate pesticide residues in fruits and vegetables.

关 键 词：高效液相色谱-串联质谱 氨基甲酸酯农药 残留 果蔬 分散固相萃取法 

分 类 号：R155.54[医药卫生—营养与食品卫生学]