高效液相色谱-串联质谱法测定鸡蛋中三聚氰胺残留

目的]建立快速测定鸡蛋中三聚氰胺残留的高效液相色谱-串联质谱方法。方法]采用1%三氯乙酸-甲醇（体积比1∶1）提取鸡蛋样品中的三聚氰胺残留,然后用PCX柱净化,用反相液相色谱分离,以液相色谱-串联质谱仪测定,外标法定量。结果]该法对三聚氰胺的线性范围为20～400μg/kg,相关系数r2=0.998 5;在50、100、200μg/kg 3个添加水平范围内的回收率为87.0%、96.8%、94.4%,检测限为3μg/kg,定量限为10μg/kg。结论]该方法简便快速,灵敏度高,重现性好,选择性强,非常适合鸡蛋中三聚氰胺药物残留的确证和定量测定。

Determination of Melamine Residue in Egg by High-performance Liquid Chromatographic Method-Tandem Mass Spectrometry

Objective]An high-performance liquid chromatographic method with tandem mass spectrometry(HPLC-MS/MS) was developed for the determination of melamine residues in eggs.Method]The melamine residue was extracted with 1% trichloroacetic acid-methanol(V/V=1∶1),and cleaned-up with PCX solid phase extraction column.The solution was separated on a RP-HPLC column and detected by HPLC-MS/MS with positive electrospray ionization(ESI+) in multiple reaction monitoring(MRM) mode.Quantitation was carried out using an external standard method.Result]The standard curves for all compounds were linear over the concentration range of 20-400 μg/kg with correlation coefficients(r2) of 0.998 5;The recoveries of melamine from egg samples spiked with the concentration levels at 50,100,200 μg/kg were range of 87.0%,96.8% and 94.4%.The limit of detection for the method was 3 μg/kg.The limit of quantification for the method was 10 μg/kg.Conclusion]The established method was of simplicity,rapidity,high sensitivity,good reproducibility and better selectivity,which was quite fit for identification and determination of melamine in eggs.