食品科学 ›› 2013, Vol. 34 ›› Issue (10): 289-293.doi: 10.7506/spkx1002-6630-201310064

• 分析检测 • 上一篇    下一篇

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

丁 俭,李培武,李光明,王秀嫔,马 飞   

  1. 1.中国农业科学院油料作物研究所,湖北 武汉 430062;2.农业部油料作物生物学与遗传育种重点实验室,湖北 武汉 430062;3.农业部生物毒素检测重点实验室,湖北 武汉 430062;4.农业部油料产品质量安全风险评估实验室,湖北 武汉 430062;5.农业部油料及制品质量监督检验测试中心,湖北 武汉 430062
  • 收稿日期:2012-02-26 修回日期:2013-04-07 出版日期:2013-05-25 发布日期:2013-05-07
  • 通讯作者: 李培武 E-mail:peiwuli@oilcrops.cn

Determination of Aflatoxin M1 in Milk by High Performance Liquid Chromatography Using On-line Solid Phase Extraction

DING Jian,LI Pei-wu,LI Guang-ming,WANG Xiu-pin,MA Fei
  

  1. 1. Institute of Oil Crops Research, Chinese Academy of Agricultural Sciences, Wuhan 430062, China;
    2. Key Laboratory of Biology and Genetic Improvement of Oil Crops, Ministry of Agriculture, Wuhan 430062, China;
    3. Key Laboratory of Detection for Mycotoxins, Ministry of Agriculture, Wuhan 430062, China;
    4. Laboratory of Risk Assessment for Oilseeds Products (Wuhan), Ministry of Agriculture, Wuhan 430062, China;
    5. Quality Inspection and Test Center for Oilseeds Products, Ministry of Agriculture, Wuhan 430062, China
  • Received:2012-02-26 Revised:2013-04-07 Online:2013-05-25 Published:2013-05-07
  • Contact: Pei-Wu Li E-mail:peiwuli@oilcrops.cn

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。

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

Abstract:

Objective: A novel method was developed for the determination of aflatoxin M1 in 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 M1 in milk.

Key words: on-line soild phase extraction, milk, high performance liquid chromatography, aflatoxin M1