气相色谱-串联质谱法测定5种植物源性食品中氯酞酸和草芽畏残留量

Determination of chlorthal and 2,3,6-trichlorobenzoic acid residues in 5 kinds of plant-origin food by gas chromatography-tandem mass spectrometry

中文关键词:  气相色谱-串联质谱法  氯肽酸  草芽畏  水果蔬菜  茶叶  粮谷  花生油

英文关键词:gas chromatography-tandem mass spectrometry  chlorthal  2,3,6-trichlorobenzoic acid  fruits and vegetables  tea  grain  peanut oil

中文摘要:

      目的 建立气相色谱-串联质谱法测定水果、蔬菜、茶叶、粮谷及花生油等植物源食品中氯酞酸和草芽畏两种农药残留的分析方法。方法 针对非油基质样品, 选取柚子、生菜、茶叶及小麦粉样品, 经2%甲酸乙腈溶液提取, 三甲基硅烷化试剂衍生, MAS-Q盐包吸附色素等杂质, 再经HLB柱净化的前处理方法; 针对含油基质, 选取花生油样品, 经甲醇提取, 三甲基硅烷化试剂衍生, 再经HLB柱净化。净化后样品用气相色谱-串联质谱仪进行检测。结果 为消除基质效应影响, 补偿前处理提取过程中的损失, 采用过程标准校正法, 两种农药在不同基质样品中呈现良好的线性关系, 相关系数均大于0.99。在0.01、0.02、0.05 mg/kg加标水平下, 两种农药在不同基质中的回收率均在93.6%~113.6%之间, 相对标准偏差在0.9%~9.8%之间 (n=6)。结论 该方法灵敏度高, 选择性好, 在水果、蔬菜、粮谷、乃至茶叶、花生油等复杂基质中, 氯酞酸和草芽畏的定量限均可达到0.01 mg/kg, 满足GB 2763—2021《食品安全国家标准 食品中农药最大残留限量》临时限量的要求。

英文摘要:

      Objective To establish a gas chromatography-tandem mass spectrometry method for the determination of chlorthal and 2,3,6-trichlorobenzoic acid residues in fruits, vegetables, tea, grain and peanut oil. Methods For non-oil matrices such as fruits and vegetables, tea and grains, pomelo, lettuce, tea and wheat flour samples were selected and extracted by 2% acetonitrile formate solution, derived by trimethylsilanization reagent, MAS-Q salt package was applied to adsorb pigment and other impurities, and then purified by HLB column. For oil matrices, the peanut oil sample was selected and extracted by methanol, derived by trimethylsilanization reagent, and then purified by HLB column. The purified samples were detected by gas chromatography-tandem mass spectrometry. Results By applying procedural standard calibration method to eliminate matrix effect and to compensate for losses during extraction, the 2 kinds of pesticides showed a good linearity in different matrices, and the correlation coefficient was greater than 0.99. At 0.01, 0.02 and 0.05 mg/kg concentration levels, the recovery of the 2 kinds of pesticides in different matrices ranged from 93.6% to 113.6%, and the relative standard deviation were from 0.9% to 9.8% (n=6). Conclusion The method has a high sensitivity and good selectivity. In matrices of fruits and vegetables, grains, even tea, and peanut oil, the limits of quantitative of chlorthal and 2,3,6-trichlorobenzoic acid can reach to 0.01 mg/kg, meeting the requirements of GB 2763—2021 National food safety standards-Maximum residue limits for pesticides in food.