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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 method for the determination of melamine in melamine tableware by liquid chromatography-tandem electrospray ionization mass spectrometry (LC-ESI MS / MS) was developed. A strong cation exchange column was used with a mobile phase of acetonitrile-10 mmol / L ammonium acetate / acetic acid buffer (pH 4.0) (40:60, volume ratio). Qualitative and quantitative analysis of melamine was performed with multiple reaction monitoring. The concentration of melamine in water, 3% acetic acid and 10% ethanol mimics showed a good linear relationship between the peak area and the mass concentration of melamine in the range of 3.00-130.00 μg / L. The detection limit (S / N = 3) And 1.00μg / L respectively. The linear range of the proposed method was 5.00-130.00μg / L in olive oil and isooctane mimics and the detection limit (S / N = 3) was 3.00μg / L. The recoveries of samples at the spiked levels of 10.00, 50.00 and 80.00 μg / L were 98% -104% with RSD of 3.0% -3.6%. The method has the advantages of simple pretreatment, high sensitivity and strong anti-interference ability, and can meet the detection requirement of melamine in melamine tableware and related products.