QuEChERS-气相色谱-串联质谱法同时测定高粱中16种农药残留

Simultaneous determination of 16 kinds of pesticides residues in sorghum by QuEChERS-gas chromatography-tandem mass spectrometry

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

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

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)同时检测高粱中16种农药残留的分析方法。方法 高粱粉末加水浸润后, 加入WondaPak QuEChERS提取盐试剂包Ⅱ均质提取, 取上清液加入WondaPak QuEChERS净化管Ⅲ净化, 氮吹近干, 定容至1 mL, 基质内标法定量测定。结果 在0.05~1.00 μg/mL范围内, 各农药的线性关系良好, 相关系数(r2)均不小于0.998, 方法检出限为0.00124~0.65400 μg/kg。在0.01、0.10和0.50 mg/kg 3个加标水平浓度下, 加标平均回收率为78.54%~102.22%, 相对标准偏差(relative standard deviations, RSDs)为1.23%~9.52% (n=6)。结论 该方法具有前处理操作简单、重复性好、灵敏度高、简化样品前处理过程、降低分析成本等优势, 适用于高粱中常用农药的高灵敏度快速检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of 16 kinds of pesticides residues in sorghum by QuEChERS-gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods After the sorghum powder was soaked in water, the WondaPak QuEChERS extraction salt reagent pack II was added for homogenization extraction, the supernatant was added to WondaPak QuEChERS purification tube III for purification, the nitrogen was blown nearly dry, the volume was fixed to 1 mL, and the matrix internal standard method was used for quantitative determination. Results Each pesticide has good linear relationship in the range of 0.05?1.00 μg/mL, the correlation coefficients (r2) of the linear regression equations were all greater than or equal to 0.998, and the limits of detection of the method were 0.00124-0.65400 μg/kg. At 3 levels of 0.01, 0.10 and 0.50 mg/kg, the average recoveries of the addition were 78.54%?102.22%, and the relative standard deviations (RSDs) were 1.23%?9.52% (n=6). Conclusion This method has the advantages of simple pretreatment operation, good reproducibility, high sensitivity, simplified sample preparation process, and reduced analysis cost, etc, it is suitable for high sensitivity and rapid detection of common pesticides in sorghum.