基于PRiME-HLB的超高效液相色谱-串联质谱法测定蔬菜中43种农药残留

Determination of 43 kinds of pesticide residues in vegetables by ultra performance liquid chromatography-tandem mass spectrometry based on PRiME-HLB

中文关键词:  QuEChERS  PRiME-HLB  蔬菜  超高效液相色谱-串联质谱法  农药残留

英文关键词:QuEChERS  PRiME-HLB  vegetables  ultra performance liquid chromatography-tandem mass spectrometry  pesticide residues

中文摘要:

      目的 建立基于PRiME-HLB的超高效液相色谱-串联质谱法测定蔬菜中43种农药残留的分析方法。 方法 称取10 g蔬菜样品(西红柿、黄瓜、菠菜、红辣椒、生姜、韭菜、葱、土豆), 以乙腈为溶剂, 加入QuEChERS盐包(4 g无水MgSO4、1 g NaCl、0.5 g柠檬酸氢二钠、1 g柠檬酸钠)进行萃取, 采用PRiME-HLB固相小柱免活化净化, 与超高效液相色谱-串联质谱技术联用, 实现蔬菜中多农药残留的分析测定。结果 PRiME-HLB固相小柱能够有效降低蔬菜样品中复杂基质对农药残留检测的影响, 其中70%的农药化合物属于弱基质效应; 43种农药分子在5~200 μg/L的质量浓度范围内具有良好的线性关系, 相关系数(r2)均大于0.993; 在实际样品中的加标回收率为55%~122%, 相对标准偏差为0.2%~19.1%; 最低定量限均小于6 μg/kg。结论 该方法操作灵敏、准确可靠, 能够用于不同种类蔬菜中多种农药残留量的准确测定。

英文摘要:

      Objective To establish a method for the determination of 43 kinds of pesticide residues in vegetables by ultra performance liquid chromatography-tandem mass spectrometry based on PRiME-HLB. Methods The 10 g of vegetable samples (tomato, cucumber, spinach, red pepper, ginger, leek, onion, potato) were weighed and extracted with QuEChERS salt (4 g anhydrous MgSO4, 1 g NaCl, 0.5 g disodium hydrogen citrate, 1 g sodium citrate) in acetonitrile as solvent. Using PRiME-HLB solid phase small column without activation purification, combined with ultra performance liquid chromatography-tandem mass spectrometry, the determination of multiple pesticide residues in vegetables was realized. Results PRiME-HLB solid phase column could effectively reduce the influence of complex matrix on the detection of pesticide residues in vegetable samples, and 70% of pesticide compounds belonged to weak matrix effect. The 43 kinds of pesticide molecules showed good linear relationships in the mass concentration range of 5?200 μg/L, and the correlation coefficients (r2) were all greater than 0.993. The recoveries were 55%?122% and the relative standard deviations were 0.2%?17.0%. The minimum limits of quantification were all less than 6 μg/kg. Conclusion This method is sensitive, accurate and reliable, and consequently has a great application for the determination of multiple pesticide residues in different kinds of vegetables.