LC-ESIMS／MS测定蜜胺餐具中三聚氰胺的迁移量

Determination of Melamine Migration in Melamine Tableware by LC-ESI MS/MS

建立了液相色谱串联电喷雾正离子源质谱(LC-ESI MS/MS)检测蜜胺餐具中三聚氰胺迁移量的方法。采用强阳离子交换柱,流动相为乙腈-10 mmol/L乙酸铵/乙酸缓冲溶液(pH4.0)(40∶60,体积比),以多反应离子监测对三聚氰胺做定性定量分析。在水、3%乙酸、10%乙醇模拟物中,三聚氰胺在3.00~130.00μg/L质量浓度范围内,目标物的峰面积和质量浓度呈良好线性关系,检出限(S/N=3)为1.00μg/L;而其在橄榄油和异辛烷模拟物中的线性范围为5.00~130.00μg/L,检出限(S/N=3)为3.00μg/L。在10.00、50.00、80.00μg/L加标水平下的样品回收率为98%~104%,RSD为3.0%~3.6%。该方法前处理简单,灵敏度高,抗干扰能力强,可满足蜜胺餐具及相关产品中三聚氰胺迁移量的检测需求。

A liquid chromatography - electrospray ionization tandem mass spectrometric （ LC - ESI MS/MS） method was developed for the sensitive and selective determination of melamine migration in food contact materials, melamine tableware. The separation was performed on a strong cation exchange column using acetonotrile - 10 mmol/L NH4Ac/HAc （pH --4.0） （40 ： 60, by volume） as mobile phase at 35 ℃. The determination of melamine in melamine tableware sample was carried out by ESI MS/MS system under the muti-reaction monitering mode （MRM）. The result indicated that the calibration curves were linear over melamine concentration in the range of 3.00 - 130.00 I.~g/L for different simulant solutions with LODs （ S/N = 3 ） of I. 00 - 3.00 I^g/L. The average recoveries at three spiked concentration levels of 10. 00, 50. 00, 80. 00 txg/L were in the range of 98% - 104% with relative standard deviations of 3.0% - 3.6% . With the advantages of simple sample preparation, high sensitivity and strong anti-interference capacity, the method could meet the requirements for determination of melamine migrantion from relevant products.