高效液相色谱法同时测定功能食品中6种违禁成分

目的 建立同时测定功能食品中去甲伪麻黄碱、伪麻黄碱、安非拉酮、士的宁、芬氟拉明和西地那非的高效液相色谱-二极管阵列检测法(HPLC-DAD)。 方法 样品经2%甲酸-水超声提取,强阳离子交换(SCX)固相萃取净化,0.05 mol/L磷酸二氢钾(pH3.0)-乙腈为流动相,C₁₈柱分离。色谱峰保留时间结合峰内光谱比较定性,外标标准曲线法定量。 结果 以本方法建立的6种化合物标准曲线线性相关系数均大于0.999,日内相对标准差为6.25%~8.19%,日间相对标准差为6.61%~10.8%,平均加标回收率为80.5%~110.0%,检出限为15.9~66.5 μg/kg。 结论 本研究建立的方法简便、灵敏度和检出限符合功能食品中违禁成分检测、分析成本低,可用于不同剂型功能食品中6种违禁添加成分的测定。

Simultaneous Determination of Six Adulterants in Functional Foods by High Performance Liquid Chromatography with Diode Array Detection

Objective To establish a method for simultaneous determination of six adulterants including norpseudoephedrine (NPE), pseudoephedrine (PSE), amfepramone (AMF), strychnine (STR), fenfluramine (FEN) and sildenafil (SIL) in functional foods by high performance liquid chromatography with diode array detection (HPLC-DAD). Methods Food samples were treated with 2% formic acid ultrasonically, and then the extracts were cleaned-up with solid phase extraction (SPE) with strong cation exchange cartridges (SCX). The sample solution was separated on a C₁₈ column with the mobile phase composed of 0.05 mol/L potassium dihydrogen phosphate (pH3.0) and acetonitrile. The qualitative analysis was accomplished with spectral and retention times of the chromatographic peaks. The external standard curves were established for quantification of the adulterants. Results The linear correlation coefficients of the 6 chemicals were greater than 0.999. The intraday RSDs were 6.25%-8.19% and the interday RSDs were 6.61%-10.8% with the average recoveries of 80.5%-110.0%. The detection limits of the method were 15.9-66.5 μg/kg. Conclusion The method is simple, sensitive and inexpensive and is suitable to the determination of the 6 chemicals in functional foods.