高效液相色谱法检测食品接触产品中的三聚氰胺及其衍生物的迁移量

摘要

A novel High-performance liquid chromatographic method of determining monomer migration of melamine (MEL) and its derivatives including ammeline (ANE), ammelide (ADE) and cyanu-ric acid (CYA) was developed. Samples were immersed in simulants (H2O, 4% acetic acid, 10% ethanol), and then kept in incubator at 70 ℃ in a duration of 4 h. The immersed solutions were injected into HPLC column before the penetration through a 0. 45-μm microporous membrane. The separation was performed on a Phenomenex Luna NH2 column at 30 ℃ and the mobile phase of acetoni-trile (5 mmol/L) with PBS (pH =6. 5)(75:25, V/V) of isocratic elution was pumped at a flow rate of 1. 0 mL/min with DAD detection at 205 and 214 nm. Under the optimum conditions, the calibration curves were linear from 0. 5 to 10 mg/L with LODs (S/N = 3) of 0. 06, 0. 08, 0. 12 and 0. 15 mg/L for MEL, ANE, ADE and CYA, respectively. The method provided recoveries of 96. 4% - 101. 6% in the spiked concentration of 1. 0 mg/L, and the RSD of the peak height was between 2. 8% and 4. 4%. The satisfied experimental results indicated that the proposed method can be directly used for the determination of monomer migration of melamine and its derivatives in food contact material conveniently, rapidly and accurately.%建立了高效液相色谱同时检测三聚氰胺(MEL)及其衍生物——三聚氰酸二酰胺(ANE)、三聚氰酸一酰胺(ADE)和三聚氰酸(CYA)单体迁移量的方法.样品分别采用水、4％乙酸、10％乙醇作为食品模拟物,在70℃浸泡4h,浸泡液过0.45μm微孔薄膜后进入色谱柱.色谱分离采用Luna NH2柱,柱温:30℃,流动相为V(乙腈):V((5 mmol/L PBS缓冲溶液,pH 6.5)=75:25,流速:1.0 mL/min; DAD检测波长为205和214 nm.在此优化条件下,MEL,ANE,ADE和CYA的浓度在0.5～10 mg/L范围内与其峰面积的线性关系良好,检出限分别为0.06,0.08.0.12和0.15 mg/L(S/N=3).在1.0 mg/L的添加水平下,MEL,ANE,ADE和CYA的平均回收率在96.4％～101.6％之间,相对标准偏差在2.79％～4.39％之间.结果表明,本方法可简便、快速、准确地同时测定食品接触产品中三聚氰胺及其衍生物的迁移量.