液质法测定婴幼儿米粉中壬基酚和丙烯酰胺

Determination of Nonylphenol and Acrylamide in Infant Rice Flour by LC-MS/MS

建立高效液相色谱-质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)测定婴幼儿营养米粉中壬基酚和丙烯酰胺残留的检测方法。样品先经水溶解,再用无水乙醇超声提取,减压浓缩后复溶于5 m L 10%甲醇水溶液。以MGⅢ-C18色谱柱(4.6 mm×150 mm,5μm)分离,流动相为甲醇和水(梯度洗脱),流速0.20 m L/min。同位素内标定量。在该优化条件下,定量限分别为1.5μg/kg和10μg/kg,方法回收率为90.2%~103.1%,相对标准偏差(relative standard deviation,RSD)为3.80%~4.87%。结果表明该方法前处理简单,灵敏度高,适合于婴幼儿营养米粉中壬基酚和丙烯酰胺残留的同时快速检测。

A new liquid chromatography-tandem mass spectrometry（LC-MS/MS）method was established for the simultaneous determination of residues of nonylphenol and acrylamide in infant nutrient rice flour. Samples were ultrasonicated with ethanol. The extract was concentrated by evaporation and redissolved in 5 m L of water containing 10 % methanol. The chromatographic separation was carried out on a MGⅢ-C18 column（4.6 mm ×150 mm,5 μm） using a mobile phase made up of methanol and water by gradient elution at a flow rate of0. 20 m L/min. Internal standard method was used for quantitative analysis. The limits of quantification were1.5 μg/kg and 10 μg/kg,respectively. The average spike recoveries of the method ranged from 90.2 % to103.1 % with relative standard deviations（RSD）of 3.80 %-4.87 %.This method is proved to be simple,rapid,sensitive and effective for simultaneously determining residues of nonylphenol and acrylamide in infant nutrient rice flour.