QuEChERS-超高效液相色谱-QDa质谱法快速测定白菜与油菜中15种氨基甲酸酯类农药及代谢物残留

Residue determination of 15 carbamates and their metabolites in Chinese cabages and pakchoi by QuEChERS-ultra high performance liquid chromatography-QDa mass spectrometry

基于QuEChERS方法,采用乙腈提取目标物,采用新型净化装置多功能针式过滤器净化,以CORTECS~？T3色谱柱（3.0 mm×150 mm,2.7μm）进行液相分离,通过超高效液相色谱-QDa质谱（UPLC-QDaMS）单离子扫描模式进行快速测定分析,建立了白菜与油菜中15种氨基甲酸酯类农药及其代谢物残留的快速分析方法,单个样品处理分析过程不超过30 min。结果表明：在0.001～0.1 mg/L范围内,白菜与油菜中15种氨基甲酸酯类农药及代谢物的质量浓度与对应的峰面积间线性关系良好（r〉0.99）。在0.01～0.2mg/kg添加水平下,回收率处于68%～120%之间,相对标准偏差均小于15%（n=3）,方法检出限范围（LOD,S/N≥3）为0.001～0.004 mg/kg,定量限（LOQ,S/N≥10且回收率处于60%～120%之间）处于0.005～0.01 mg/kg之间。该方法准确、快速、稳定,适合基层实际检测需要。

A rapid method for the residue determination of 15 carbamates and their metabolites in Chinese cabage and pakchoi by ultra high performance liquid chromatography-QDa mass spectrometry（UPLC-QDaMS） was established. Sample pretreatment was based on the QuEChERS method. The target substance was extracted with acetonitrile and purified with multi-functional needle filter（MFF）.Column CORTECS~？ T3（3.0 mm × 150 mm, 2.7 μm） was used in the chromatographic separation, and QDa mass spectrometry with single ion scan mode analysis was used to detect pesticides. The results showed that a good linear relationships（r 0.99） in two matrices were obtained for 15 pesticides and their metabolites in the range of 0.001-0.1 mg/L. The recoveries of the target compounds in two matrices were both 68%-120%, and the RSDs were both less than 15%（n = 3）. The limits of detection（LOD, S/N≥3） ranged from 0.001 to 0.004 mg/kg. The limits of quantitation（LOQ, S/N≥10 and recovery in the range of 60%-120%） were 0.005-0.01 mg/kg. These results indicated that the developed method was accurate, rapid and stable, and suitable for the detection requirements in the grass-roots unit.