A reliable and sensitive method was developed for simultaneous determination of glyphosate and glufosinate in various food products by liquid chromatography-tandem mass spectrometry. Based on extraction, derivatization with 9-fluorenylmethylchloroformate and purification on solid phase extraction column, quantification was done by using isotopic-labeled analytes as internal standard and calibration in matrix. Good selectivity and sensitivity were achieved with a limit of quantification of 5 μg/kg. The recoveries of these two pesticides ranged from 91% to 114% with inter-day and relative standard deviation of 3.8–6.1% in five matrices of cereal group spiked at 5, 10, and 20 μg/kg. An accuracy profile was performed for method validation, demonstrating the accuracy and precision of the method for the studied food groups. The verification results in expanded food groups indicated extensive applicability for the analysis of glyphosate and glufosinate. Finally, the developed method was applied to analyze 136 food samples including milk-based baby foods from the French Agency for Food, Environmental and Occupational Health & Safety. Glyphosate residues were detected in two breakfast cereal samples (6.0 and 34 μg/kg). Glufosinate residues were found in a sample of boiled potatoes (9.8 μg/kg). No residues were detected in the other samples, including milk-based baby foods with limits of detection ranging from 1 to 2 μg/kg. The method has been applied for routine national monitoring of glyphosate and glufosinate in various foods.

建立了一种可靠且灵敏的方法，可通过液相色谱-串联质谱法同时测定各种食品中的草甘膦和草铵膦。在萃取，9-芴基甲基氯甲酸酯衍生化和在固相萃取柱上纯化的基础上，使用同位素标记的分析物作为内标物进行定量，并在基质中进行校准。获得了良好的选择性和灵敏度，定量限为5μg/ kg。两种谷物中五种谷物浓度分别为5、10和20μg/ kg的日间和相对标准偏差为3.8–6.1％，这两种农药的回收率在91％至114％之间。进行了准确性简档以进行方法验证，证明了所研究食品组方法的准确性和精确性。扩大食品类别的验证结果表明，草甘膦和草铵膦的分析具有广泛的适用性。最后，该改进的方法被用于分析136种食品样本，包括来自法国食品，环境与职业健康与安全局的牛奶类婴儿食品。在两个早餐谷物样品（6.0和34μg/ kg）中检测到草甘膦残留物。在煮土豆样品中发现了草铵膦残留物（9.8μg/ kg）。在其他样品（包括牛奶基婴儿食品）中未检测到残留，检测限为1至2μg/ kg。该方法已被用于常规监测各种食品中的草甘膦和草铵膦。该开发的方法用于分析136种食品样本，包括法国食品，环境与职业健康与安全局的牛奶类婴儿食品。在两个早餐谷物样品（6.0和34μg/ kg）中检测到草甘膦残留物。在煮土豆样品中发现了草铵膦残留物（9.8μg/ kg）。在其他样品（包括牛奶基婴儿食品）中未检测到残留，检测限为1至2μg/ kg。该方法已被用于常规监测各种食品中的草甘膦和草铵膦。该开发的方法用于分析136种食品样本，包括法国食品，环境与职业健康与安全局的牛奶类婴儿食品。在两个早餐谷物样品（6.0和34μg/ kg）中检测到草甘膦残留物。在煮土豆样品中发现了草铵膦残留物（9.8μg/ kg）。在其他样品（包括牛奶基婴儿食品）中未检测到残留，检测限为1至2μg/ kg。该方法已被用于常规监测各种食品中的草甘膦和草铵膦。在煮土豆样品中发现了草铵膦残留物（9.8μg/ kg）。在其他样品（包括牛奶基婴儿食品）中未检测到残留，检测限为1至2μg/ kg。该方法已被用于常规监测各种食品中的草甘膦和草铵膦。在煮土豆样品中发现了草铵膦残留物（9.8μg/ kg）。在其他样品（包括牛奶基婴儿食品）中未检测到残留，检测限为1至2μg/ kg。该方法已被用于常规监测各种食品中的草甘膦和草铵膦。