反相高效液相色谱法测定乳品及乳制品中的黄曲霉毒素M1
RP-HPLC Determination of Aflatoxin M1 in Milk and Its Products
摘 要
采用反相高效液相色谱测定乳品及乳制品中黄曲霉毒素M1(AFM1)的含量.样品经氯仿提取,过硅胶固相萃取柱净化,用氯仿-丙酮(1+1)混合溶液将黄曲霉毒素M1从固相萃取柱上洗脱下来.以ZORBAX SB C18色谱柱为分离柱,水和乙腈为流动相梯度淋洗,用荧光检测器检测,外标法定量.黄曲霉毒素M1在1.0~25 μg·L-1质量浓度范围内与其峰面积呈线性关系,检出限(3S/N)为0.05 μg·kg-1.应用此法测定了牛奶和乳粉中AFM1的含量,并测得其平均回收率分别在76.0%~80.0%和76.7%~90.8%之间,相对标准偏差(n=6)均小于7.0%.
黄曲霉毒素M1
荧光检测器
RP-HPLC
Aflatoxin M1
Fluorescence detector
Abstract
RP-HPLC was applied to the determinations of aflatoxin M1 (AFM1) in milk and its products.The sample was extracted with chloroform,and purified by passing through silica gel solid phase extraction column,and AFM1 was eluted from the SPE column with a mixed solution of chloroform and acetone (1+1).The eluate was separated by gradient elution with acetonitrile solution of different concentration from ZORBAX SB C18 column,and their contents determined by fluorescence detector.Linear relationship between values of peak area and mass concentration of AFM1 was obtained in the range of 1.0-25 μg·L-1,with detection limit (3S/N) 0.05 μg·kg-1.The proposed method was used in the analysis of milk and milk powder for their contents of AFM1 and values of recovery found by standard addition method were in the range of 76.0%-80.0% and 76.7%-90.8% respectively,and values of RSD′s (n=6) found were less than 7.0%.
中图分类号 O657.7
所属栏目 工作简报
基金项目
收稿日期 2008/10/7
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备注张春艳(1969-),女,内蒙古呼和浩特市人,高级工程师,硕士,从事食品检测及技术研究.
引用该论文: ZHANG Chun-yan,PAN Guo-qing,LIU Lai-jun,BAI Guo-tao,ZHANG Wei,LIU Zhong-xue. RP-HPLC Determination of Aflatoxin M1 in Milk and Its Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(9): 1032～1034
张春艳,潘国卿,刘来俊,白国涛,张伟,刘中学. 反相高效液相色谱法测定乳品及乳制品中的黄曲霉毒素M1[J]. 理化检验－化学分册, 2009, 45(9): 1032～1034
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参考文献
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【2】LIU Ling,DANIELS J M,STEWART R K,et al.In vitro prostaglandin H synthase and monooxygenase mediated binding of aflatoxin B1 to DNA in guinea-pig tissue microsomes[J].Carcinogenesia,1990,11:823-827．
【3】VELASCO R M L,DELSO M M C.ELISA and HPLC determination of the occμrrence of aflatoxin M1 in raw cow′s milk[J].Food Addit Contam,2003,20:276-280．
【4】张东升,赵晓联,赵春城,等.黄曲霉毒素M1的危害、污染现状及检测方法进展[J].中国卫生检验杂志,2004,6:266-269．
【2】LIU Ling,DANIELS J M,STEWART R K,et al.In vitro prostaglandin H synthase and monooxygenase mediated binding of aflatoxin B1 to DNA in guinea-pig tissue microsomes[J].Carcinogenesia,1990,11:823-827．
【3】VELASCO R M L,DELSO M M C.ELISA and HPLC determination of the occμrrence of aflatoxin M1 in raw cow′s milk[J].Food Addit Contam,2003,20:276-280．
【4】张东升,赵晓联,赵春城,等.黄曲霉毒素M1的危害、污染现状及检测方法进展[J].中国卫生检验杂志,2004,6:266-269．
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