QuEChERS-气相色谱-串联质谱法测定红糖中172种农药残留

Determination of 172 kinds of pesticide residues in brown sugar by QuEChERS-gas chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  农药残留  气相色谱-串联质谱法  红糖

英文关键词:QuEChERS  pesticide residues  gas chromatography-tandem mass spectrometry  brown sugar

中文摘要:

      目的 建立QuEChERS-气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)检测红糖中172种农药残留的方法。方法 样品加入超纯水充分溶解后经正己烷高速匀浆提取, 氮吹浓缩, QuEChERS法净化, 采用GC-MS/MS检测技术, 以分段时间选择反应监测模式(selective reaction monitoring, SRM)模式进行数据采集, 配制基质匹配曲线及溶剂曲线进行定量检测。结果 172种农药在10~200 ng/mL质量浓度的线性范围内线性关系良好, 线性相关系数在0.9962~0.9999之间, 定量限为0.01 mg/kg, 在1、2、10倍定量限的浓度下各进行6次重复的加标实验, 平均加标回收率在71.0%~113.0%之间, 相对标准偏差为0.49%~17.00% (n=6)。结论 该方法利用QuEChERS法净化, 一次进样可以检测上百种农药, 具有快速、简便、高通量、经济等特点, 适用于红糖中多种农药残留的检测。

英文摘要:

      Objective To establish the detection of 172 kinds of pesticide residues in brown sugar by QuEChERS-gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The samples were fully dissolved in ultrapure water and extracted by high-speed homogenization of n-hexane, nitrogen blowing and concentration, and purified by QuEChERS method, and the data was collected in selective reaction monitoring mode by GC-MS/MS detection technology, and quantitatively detected by matrix curve and solvent curve. Results The 172 kinds of pesticides had a good linear relationship in the linear range of 10–200 ng/mL, and the linear correlation coefficient was between 0.9962 and 0.9999, the limit of quantification of the method was 0.01 mg/kg, performed 6 repeated spiked experiments at concentrations 1, 2, and 10 times the limit of quantification each, the recovery rate of spikes was between 71.0%–113.0%, and the relative standard deviation (n=6) was 0.49%–17.00%. Conclusions This method can detect hundreds of pesticides in one injection, which is fast, simple, high-throughput and economical, and is suitable for the detection of a variety of pesticide residues in brown sugar.