柱前衍生-高效液相色谱法同时测定乳及乳制品中5种黄曲霉毒素

Determination of five aflatoxin residues in milk and dairy products using high performance liquid chromatography coupled with pre-column derivatization

中文关键词:  柱前衍生  高效液相色谱法  乳  乳制品  黄曲霉毒素

英文关键词:pre-column derivatization  high performance liquid chromatography  milk  dairy products  aflatoxin

中文摘要:

      目的 建立柱前衍生-高效液相色谱法同时测定乳及乳制品中黄曲霉毒素M1、G1、B1、G2和B2残留的分析方法。方法 样品用乙腈作为提取溶剂辅以超声波提取、离心, 上清液浓缩至近干, 加入0.25 mL三氟乙酸在50 ℃的温度下衍生15 min后氮吹浓缩近干。采用Thermo scientific Hypersil Green PAH(4.6 mm×250 mm i.d., 5 μm)色谱柱, 乙腈和水作为流动相, 激发波长为 367 nm, 发射波长为436 nm荧光检测。结果 5种黄曲霉毒素在0.20~50.0 μg/L范围内具有良好的线性关系(0.9991~0.9998), 检出限为0.05~0.08 μg/L。在0.50 μg/kg、1.0 μg/kg和2.0 μg/kg三个添加水平的平均回收率为77.6%~122.7%, 85.8%~112.7%和89.7%~115.6%; 相对标准偏差(RSD)均小于8.92%。结论 与其他方法相比, 本法具有简便、灵敏、准确和可重复等优点, 适合乳及乳制品中5种黄曲霉毒素残留的同时检测和定量。

英文摘要:

      Objective To establish a method of simultaneous determination of AFTM1, G1, B1, G2 and B2 residues in milk and dairy products by high performance liquid chromatography coupled with pre-column derivatization. Methods The samples were extracted with 0.25 mL acetonitrile and ultrasonic-assisted, after centrifuged and concentrated to dryness, pre-column derivatization with trifluoroacetic acid at 50 ℃ and 15 min. Chromatographic analysis was performed on Thermo scientific Hypersil Green PAH(4.6 mm×150 mm i.d., 5 μm)column eluted with an acetonitrile-water and ultraviolet detector at Ex=367 nm, Em=436 nm. Results All the five aflatoxin from 0.20 μg/L to 50.0 μg/L with an excellent linear relationship (0.9991~0.9998). The detection limits of five aflatoxin were 0.05~0.08 μg/L, and the average recoveries were 77.6%~122.7%, 85.8%~112.7% and 89.7%~115.6%, respectively, with the RSD both less 8.92%. Conclusion This method of determining five aflatoxin residues of milk and dairy products showed a more convenient operation, higher sensitivity, higher accuracy and better repeatability than other methods. This quantitative method can be applied to simultaneously determination and quantification of the five aflatoxin residues in milk and dairy products.