高效液相色谱法测定食品接触材料及制品中9种酚类物质的迁移量

Determination of Migration of 9 Phenols in Food Contact Materials by High Performance Liquid Chromatography

该文建立了苯酚、甲酚类、二甲酚类等9种酚类物质迁移量同时测定的高效液相色谱(HPLC)检测方法。采用AgilentZORBAXSB-Aq色谱柱进行分离,以甲醇-水为流动相梯度洗脱,流速1.0 mL/min,荧光检测器测定,激发波长为214 nm,发射波长为315 nm。优化了含油脂食品模拟物中9种酚类物质的提取方式,并考察了线性范围、准确度及精密度等方法性能参数。研究结果表明,含油脂食品模拟物中9种酚类物质的最佳提取溶剂为67%甲醇溶液,9种酚类物质在水基及油脂类食品模拟物中的线性相关系数(r^(2))均高于0.999,回收率为90.7%~99.8%,相对标准偏差均低于6.0%。5种水基食品模拟物中9种酚类物质的定量下限为0.07~0.10 mg/L,橄榄油中9种酚类物质的定量下限为0.15~0.20 mg/kg。方法成功应用于11批食品接触用聚碳酸酯(PC)塑料制品、15批涂层制品中9种酚类物质迁移量的测定。该方法灵敏度高、精密度好,可为食品接触材料及制品中9种酚类物质迁移量的分析提供技术支持。

A high performance liquid chromatographic(HPLC)method was established for the simultaneous determination of 9 phenols such as phenol,methyl-phenols and xylenols in food simulants.The sample was separated on an Agilent ZORBAX SB-Aq column by gradient elution,using methanol and water as mobile phase at a flow rate of 1.0 mL/min,and finally determined by fluorescence detection at an excitation wavelength of 214 nm and an emission wavelength of 315 nm.Meanwhile,the extraction method for 9 phenols in the fat-contained simulant was optimized,and the performances of the method including linearity,spiked recovery and precision were studied.Results demonstrated that 67%methanol aqueous solution was the best extraction solvent for the 9 phenols in fat simulants.The results also showed that there were good linear relationships for 9 phenols in all food simulants studied,with correlation coefficients(r^(2))higher than 0.999.The recoveries for 9 phenols at 3 spiked levels in all food simulants ranged from 90.7%to 99.8%,with relative standard deviations(RSD)all below 6.0%.The limits of quantitation(LOQs)were in the ranges of 0.07-0.10 mg/L for aqueous simulants,and 0.15-0.20 mg/kg for fat simulants.This method was successfully applied to the migration determination of 9 phenols released from 11 plastics articles(PC)and 15 coatings intended to contact with food.The method was sensitive and accurate,and was suitable for the determination of 9 phenols in food simulants.