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在线固相萃取富集-高效液相色谱法快速测定牛奶中黄曲霉毒素M1

作  者:
丁俭;李培武;李光明;王秀嫔;马飞
单  位:
中国农业科学院油料作物研究所
关键词:
在线固相萃取富集;牛奶;高效液相色谱法;黄曲霉毒素M1
摘  要:
目的:建立在线固相萃取富集-高效液相色谱法(On-line SPE-HPLC)测定牛奶中黄曲霉毒素M1.方法:固相萃取富集柱填料为SB-C18,上样溶剂和淋洗溶剂均为纯水,转移溶剂为乙腈-水(20:80,V/V),分析测定溶剂为乙腈-水(15:85,V/V).结果:黄曲霉毒素M1检测的线性方程为Y=2.52746X 0.067,相关系数为0.99906;检出限为0.04μg/kg;定量限为0.10μg/kg;基质4个水平添加回收率(n=6)在98%~105.7%;6次加标回收相对标准偏差在0.79%~2.56%.结论:此方法简便、准确、重现性好,能够满足对日常牛奶中黄曲霉毒素M1的定量检测.
单  位:
Institute of Oil Crops Research,Chinese Academy of Agricultural Sciences,Wuhan 430062,China%Key Laboratory of Biology and Genetic Improvement of Oil Crops,Ministry of Agriculture,Wuhan 430062,China%Key Laboratory of Detection for Mycotoxins,Ministry of Agriculture,Wuhan 430062,China%Laboratory of Risk Assessment for Oilseeds Products(Wuhan
关键词:
on-line soild phase extraction%milk%high performance liquid chromatography%aflatoxin M1
摘  要:
Objective: A novel method was developed for the determination of aflatoxin M1in milk by HPLC with on-line solid phase extraction(SPE).Methods: An on-line SPE column was prepared through packing SB-C18 filler in stainless column.The loading and washing solution were water,transferring solution was acetonitrile-water(20:80,V/V),and elution solution was acetonitrile-water(15:85,V/V).Results: Under optimized conditions,a linear regression equation was fitted as follows: Y = 2.52746X-0.067 with a correlation coefficient of 0.99906.The detection of limit(LOD) was 0.04 μg/kg,and the limit of quantification(LOQ) was 0.10 μg/kg.Average recovery rates for samples spiked at various levels were 98%-105.7% with RSD was 0.79%-2.56%(n = 6).Conclusion: A simple,accurate and credible method has been successfully developed for rapid determination of aflatoxin M1in milk.

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