摘要
通过对提取溶剂、净化方法及色谱质谱条件的优化建立鸡组织样品中的三聚氰胺和三聚氰酸同时测定的HPLC-MS/MS法。样品经乙腈水溶液(70:30,V/V)超声提取,正己烷脱脂,7000r/min离心后取上清液与乙腈(1:1,V/V)混匀,10000r/min离心沉淀蛋白,过滤后无需净化即可上机测定,大大缩短了样品处理时间。使用MRM模式检测和同位素内标稀释法定量,进一步提高了方法的准确性和定量线性。在1～500ng/mL范围内,目标物的峰面积与其质量浓度的线性关系良好(R2>0.999);在0.1、1、5mg/kg的添加水平,鸡组织样品三聚氰胺回收率为87.76%～107.89%,三聚氰酸回收率为87.31%～106.05%,相对标准偏差(RSD)分别为0.58%～2.78%和1.26%～4.33%;三聚氰胺和三聚氰酸的检测限(LOD)分别为4ng/g和2ng/g。结果表明,该方法简便、快速、准确,适合鸡组织中三聚氰胺和三聚氰酸的确证和定量测定。
A high performance liquid chromatography-tandem mass spectrometric（HPLC-MS/MS） method was developed for the quantification of melamine（MEL） and cyanuric acid（CYA） in chicken tissues.A sample preparation procedure comprising extraction with acetonitrile mixed with water at a ratio of 70：30（V/V）,the removal of lipids with n-hexane,centrifugation at 7000 r/min,thorough mixing of the supernatant and acetonitrile（1：1,V/V）,centrifugation at 10000 r/min for the precipitation of protein and filtration through a 0.22μm membrane but excluding clean-up was used prior to HPLC-MS/MS analysis,resulting in a great reduction of the time required for sample preparation.Multiple reaction monitoring（MRM） mode was selected and internal standard isotope dilution method was used for quantification in order to improve the accuracy and quantitative linearity of the method.Calibration curves for MEL and CYA exhibited good linearity over the concentration range from 1 to 500 ng/mL,with R2 values of both larger than 0.999.Average recoveries ranged from 87.76% to107.89% for MEL and from 87.31% to 106.05% for CYA,with relative standard deviations（RSDs） ranging from 0.58% to 2.78% for MEL and from 1.26% to 4.33% for CYA at the spike levels of 0.1,1 mg/kg and 5 mg/kg.The limits of detection（LOD） of MEL and CYA were 4 ng/kg and 2 ng/g,respectively.Therefore,this method is simple,rapid and accurate and is most suitable for the quantification of MEL and CYA in chicken tissues.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2010年第12期185-192,共8页
Food Science
基金
农业部饲料中三聚氰胺限量制定专项
