摘要
建立了一种检测乳及乳制品中黄曲霉毒素B1、M1的高效液相色谱-荧光检测（HPLC-FD）方法。样品经60%乙腈溶液提取,自制固相萃取柱净化,流出液经正己烷、三氟乙酸衍生后荧光检测器检测。考察了填料、柱容量、取样量、提取溶液和流速等对检测的影响,优化了实验条件。结果表明,黄曲霉毒素B1、M1的检测线性范围为0.40~100μg/L,线性系数为0.9991~0.9998,方法检出限为0.050μg/kg。对样品进行0.40、1.0和15μg/L 3种浓度水平的加标回收实验,回收率为53%~105%,相对标准偏差为2.6%~5.1%。该方法操作简单、灵敏度高、准确度好,可用于乳及乳制品中黄曲霉毒素B1、M1的测定。
A high performance liquid chromatography（HPLC） method was developed for the determination of aflatoxin 131 and M1 （AFB1 and AFM1 ） in milk and its products. Samples were extracted by 60 % acetonitrile and cleaned up by a homemade solid phase extraction column, and detected by liquid chromatography with fluorescence detection. The effects of the packing, column capacity, sampling amount, extraction solution and flow rate on the determination of the aflatoxin residues were investigated. Under the optimized experimental conditions,the method showed a good linearity in the range of 0.40-100 μg/L with correlation coefficients of 0. 9991 and 0. 9998 and a detection limit of 0. 050μg/kg. The new method was successfully applied to the analysis of aflatoxins in milk and its products. Recoveries of aflatoxins spiked to samples at three concentration levels of 0.40,1.0 and 15 μg/L were 53%-105% with relative standard deviations of 2.6%-5.1%. With the advantages of simplicity,sensitivity and high accuracy,the method could be applied to the determination of aflatoxin B1 and M1 in milk and its products.
出处
《分析科学学报》
CAS
CSCD
北大核心
2014年第2期251-254,共4页
Journal of Analytical Science
基金
广东检验检疫局科技计划(No.2012GDK62)
关键词
自制固相萃取柱
高效液相色谱
乳制品
黄曲霉毒素
Homemade solid phase extraction column
High performance liquid chromatography
Milkproduct
Aflatoxins
