高效液相色谱法测定纸质食品接触材料及制品中3种丙烯酰胺的残留量

Determination of 3 Acrylamide Residues in Paper-Based Food Contact Materials and Products by High Performance Liquid Chromatography

建立测定纸质食品接触材料中丙烯酰胺、N-(羟甲基)丙烯酰胺和甲基丙烯酰胺的高效液相色谱(HPLC)分析方法.分别优化了流动相、柱温和提取条件.样品经剪碎后,用超纯水超声提取.提取液经0.22μm聚四氟乙烯(PTFE)滤膜过滤后,以甲醇-水为流动相进行梯度洗脱,经Agilent 5 TC-C_(18)(2)(250 mm×4.6 mm,5μm)色谱柱分离,二极管阵列检测器测定,外标法定量.结果表明,在最优条件下,丙烯酰胺、N-(羟甲基)丙烯酰胺和甲基丙烯酰胺均在0.1~5.0 mg/L浓度范围内线性关系良好,检出限分别为0.4、0.5、0.4 mg/kg,平均加标回收率为86.7%~103.3%,相对标准偏差(RSD,n=6)为2.1%~6.7%.方法前处理简单、准确度高,填补了现有标准体系中N-(羟甲基)丙烯酰胺和甲基丙烯酰胺检测方法的空白.

A high performance liquid chromatography(HPLC)for the determination of 3 acrylamides(acrylamide,Nhydroxymethacrylamide and methacrylamide)in paper-based food contact materials and products has been established.The mobile phase,column temperature,and extraction conditions were optimized,respectively.The samples were shredded and extracted by ultrasonic extraction with ultrapure water.The extract was filtered through a 0.22μm polytetrafluoroethylene(PTFE)membrane,eluted by gradient with methanol-water as mobile phase,separated by an Agilent 5 TC-C_(18)(2)(250 mm×4.6 mm,5μm)column,determined by a diode array detector,and quantified by the external standard method.The results showed that the acrylamide,N-hydroxymethacrylamide and methacrylamide had good linear relationships in the concentration range of 0.1~5.0 mg/L,the limits of detection were 0.4,0.5,0.4 mg/kg,respectively,the average spiked recoveries rate were 86.7%~103.3%,and the relative standard deviations(RSD,n=6)were 2.1%~6.7%under the optimal conditions.The method is simple and accurate,and fills the gap in the detection methods of N-hydroxymethacrylamide and methacrylamide in the standard system.