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目的建立一种简单、快捷、同时测定食品中草铵膦、草甘膦、氨甲基膦酸残留量的离子色谱分析方法。方法样品用水提取后使用乙腈沉淀氨基酸和蛋白质,离心后取上清液依次过Dionex OnGuardⅡRP柱和Dionex OnGuardⅡAg/H柱,流出液经IonPac AS11-HC离子色谱柱(含AG11-HC保护住)分离,用KOH淋洗液自动发生器(EG)进行梯度淋洗,抑制器采用外加水模式,电导检测器检测。结果结果表明草甘膦和草铵膦在0.02~6.25 mg/L、氨甲基膦酸在2.00~62.5 mg/L范围内线性关系良好,相关系数均大于0.999,Gly、Gluf和AMPA的方法检出限分为0.047、0.033和0.520 mg/kg,定量限分为0.16、0.11和1.73 mg/kg,回收率为80.1%~109%,日内精密度(n=6)为0.91%~12.5%,日间精密度(m=5)小于10.0%。结论该方法具有净化效果好、定量准确、灵敏快速的特点,适用于食品中草铵膦、草甘膦、氨甲基膦酸残留量的检测确证,能达到GB 2763-2014的检测要求。
Objective To establish a simple, rapid and simultaneous determination of glufosinate, glyphosate, aminomethylphosphonic acid residues in food by ion chromatography. Methods After the sample was extracted with water, acetonitrile and protein were precipitated. After centrifugation, the supernatant was passed through Dionex OnGuard ⅡRP column and Dionex OnGuardⅡAg / H column, and the effluent was separated by IonPac AS11-HC column (containing AG11-HC) KOH eluent automatic generator (EG) gradient elution, suppressor using an external water mode, conductivity detector detection. The results showed that glyphosate and glufosinate had a good linearity in the range of 0.02-6.25 mg / L and aminomethylphosphonic acid in the range of 2.00-62.5 mg / L with the correlation coefficients greater than 0.999, Gly, Gluf and AMPA The limits of quantification were 0.047, 0.033 and 0.520 mg / kg, with the limits of quantitation of 0.16, 0.11 and 1.73 mg / kg and the recoveries of 80.1% -109%. The intraday precision was 0.91% ~ 12.5% Daytime precision (m = 5) is less than 10.0%. Conclusion The method has the advantages of good purification effect, accurate quantification, quick and sensitive. It is suitable for the confirmation of residues of glufosinate, glyphosate and aminomethylphosphonic acid in food and can meet the test requirements of GB 2763-2014.