QuEChERS结合超高效液相色谱-串联质谱法测定八角中222种农药及其代谢物残留

Determination of 222 kinds of pesticides and their metabolite residues in Illicium verum by QuEChERS combined with ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  QUEChERS  超高效液相色谱-串联质谱法  八角  农药残留

英文关键词:QuEChERS  ultra-high performance liquid chromatography-tandem mass spectrometry  Star anise  pesticides residues

中文摘要:

      目的 建立QuEChERS结合超高效液相色谱-串联质谱法同时测定八角中222种农药及其代谢物残留的分析方法。方法 样品粉碎后以1%乙酸乙腈溶液涡旋提取，经无水硫酸镁、氯化钠、柠檬酸钠、柠檬酸氢二钠组成的萃取盐包盐析分层，十八烷基键合硅胶、N-丙基乙二胺、石墨化碳黑和无水硫酸镁分散固相萃取净化后，应用超高效液相色谱-串联质谱法进行检测，采用电喷雾电离源正负离子同时扫描，多反应监测模式检测，基质匹配标准曲线，外标法定量?结果 222种目标农药在各自线性范围内线性关系良好，相关系数（r）均大于0.999，检出限为0.00019~0.070 mg/kg，定量限为0.00062~0.23 mg/kg，在0.025、0.05、0.125 mg/kg的添加水平下，平均回收率为60.60%~113.53%，相对标准偏差（n=6）为1.02%~7.06%。共检出32种农药，其中杀虫剂和杀菌剂检出率最高。结论 建立的方法快速准确、稳定性及重现性较好，可用于八角中222种农药残留的高通量筛查及日常检验。

英文摘要:

      ABSTRACT: Objective To establish a method for the detection of 222 pesticides and their metabolite residues in Star anise by QuEChERS combined with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods Samples were extracted by 1% acetic acid acetonitrile solution after being crushed. It was salted out and stratified by an extraction salt package consisting of anhydrous magnesium sulfate, sodium chloride, sodium citrate, and disodium hydrogen citrate, solid-phase extraction purification with octadecyl bonded silica gel (C18), N-propylethylenediamine (PSA), graphitized carbon black (GCB), and anhydrous magnesium sulfate dispersion, then the samples were detected by UPLC-MS/MS, and the electrospray ionization (ESI) source was used simultaneous scanning of positive and negative ions, detected under multiple reaction monitoring (MRM) mode, matrix-matched calibration curve, and quantified by external standard method. Results 222 kinds of target pesticides exhibited great linear relationships within their respective linear ranges, with linear correlation coefficients (r) were all greater than 0.999. The limits of detection (LODs) were in the range of 0.00019～0.070mg/kg and the limits of quantification(LOQs) were in the range of 0.00062～0.23mg/kg, with addition levels at 0.025, 0.05, and 0.125 mg/kg, the average recoveries of 222 kinds of pesticides were 60.60%~113.53%, and the relative standard deviations (RSDs) (n=6) were 1.02%~7.06%. A total of 32 pesticides were detected,among which insecticides and fungicides had the highest detection rates.