QuEChERS-气相色谱-质谱法测定3种食品中11种农药残留

Determination of 11 pesticide residues in three foods by QuEChERS method coupled with gas chromatography-mass spectrometry

中文关键词:  农药残留  食品  气相色谱-质谱法

英文关键词:pesticide residues  food  gaschromatography-mass spectrometer

中文摘要:

      目的 建立气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)结合基质匹配标准系列测定3种食品中11种农药残留的分析方法。方法 样品采用QuEChERS(Quick, Easy, Cheap, Effective, Rugged, Safty)方法, 用乙腈溶液进行提取, 经N-丙基乙二胺(primary secondary amine, PSA)、十八烷基硅烷键合硅胶(C18)和无水硫酸镁固相分散净化, 浓缩定容后用GC-MS在选择离子监测模式(select ion monitoring, SIM)下进行测定, 外标法定量。结果 净化剂含量为200 mg PSA、2 g无水MgSO4时, 11种农药残留均有较好的回收率, 最终确立了采用优化后的QuEChERS(Quick, Easy, Cheap, Effective, Rugged, Safty)方法进行前处理, GC/MS检测样品的分析方法。该方法在3种基质、3个添加水平下的回收率在72.1%~112.4%之间, 相对标准偏差均小于7.0%。结论 该方法操作简便、灵敏度高, 能够满足日常检验工作的要求。

英文摘要:

      Objective To establish a method for simultaneous determination of 11 kinds of pesticide residues in 3 kinds of foods by QuEChERS pretreatment and gas chromatography-mass spectrometry(GC-MS) combined matrix matching standard series. Methods The samples were extracted with acetonitrile solution by QuEChERS (quick, easy, cheap, effective, rugged, safety) method, purified by n-propylethylenediamine (PSA), octadecylsilane bonded silica gel (C18) and anhydrous magnesium sulfate solid-phase dispersion, and determined by GC-MS under the selected ion monitoring mode (SIM) after concentration and constant volume, and quantified by external standard method. Results 200 mg of PSA, 2 g anhydrous MgSO4, 11 kinds of pesticide residues were good recovery. Finally, the optimized QuEChERS (Quick, Easy, being inexpensive, Effective, Rugged, Safty) method for pretreatment, GC/MS method for samples analysis was established. The recovery rate of the method was 72.1%?112.4% under three substrates and three addition levels, and the relative standard deviation was less than 7.0%. Conclusion This method is easy to operate, sensitive and can meet the requirements of daily inspection.