液相色谱-串联质谱法测定牛奶中11种真菌毒素残留量
LC-MS/MS Determination of Residual Amounts of 11 Mycotoxins in Milk
摘 要
采用液相色谱-串联质谱法测定牛奶中11种真菌毒素的残留量.样品经乙腈沉淀蛋白和提取,正己烷脱脂,无水硫酸钠干燥,M160型多功能净化柱净化.以Agilent Eclipse XDB-C18色谱柱为分离柱,以不同体积比的水和甲醇混合液为流动相进行梯度洗脱,采用多反应监测模式检测.11种真菌毒素的质量分数均在4.0 μg·kg-1以内与其峰面积呈线性关系,方法的检出限(3S/N)在0.001~0.006 ng之间.加标回收率在60.1%~95.2%之间,测定值的相对标准偏差(n=6)在3.2%~9.6%之间.
牛奶
真菌毒素
LC-MS/MS
Milk
Mycotoxins
Abstract
LC-MS/MS was applied to the determination of residual amounts of 11 mycotoxins in milk.The sample was extracted and protein precipitated with acetonitrile,and then fat was removed by n-hexane,dried with anhydrous sodium sulfate,cleaned up with M160 cartridges.Agilent Eclipse XDB-C18 chromatographic column was used as stationary phase,and the mixture of methanol and water mixed in different ratio was used as mobile phase in gradient elution.Multi-reactions monitor was adopted in MS/MS.Linear relationships between values of peak area and mass fraction of the 11 mycotoxins were kept in the same range within 4.0 μg·kg-1,with detection limits (3S/N)in the range of 0.001-0.006 ng.Values of recovery found by standard addition method were in the range of 60.1%-95.2%,and values of RSD′s (n=6) in the range of 3.2%-9.6%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 浙江省重点科技创新团队“农产品安全标准与检测技术”(2010R50028)
收稿日期 2014/5/12
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备注侯建波(1983-),男,满族,内蒙古人,高级工程师,博士,研究方向为食品中药物残留分析.
引用该论文: HOU Jian-bo,XIE Wen,LI Jie,ZHU Ze-long,HE Jian-min. LC-MS/MS Determination of Residual Amounts of 11 Mycotoxins in Milk[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(5): 600～604
侯建波,谢文,李杰,祝泽龙,何建敏. 液相色谱-串联质谱法测定牛奶中11种真菌毒素残留量[J]. 理化检验－化学分册, 2015, 51(5): 600～604
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参考文献
【1】Council for Agricultural Science and Technology.Mycotoxins: risks in plant,animal and human systems[M].Ames: Council for Agricultural Science and Technology,2003.
【2】GB 2761-2011食品中真菌毒素限量[S].
【3】Commission Regulation (EC) No 1881/2006Setting maximum levels for certain contaminants in foodstuffs[S].
【4】陈瑞春,段文仲,吕红英,等.免疫亲和层析净化-高效液相色谱法同时测定牛奶和奶粉中黄曲霉毒素B1、B2、G1、G2、M1、M2[J].食品科技,2011,36(8):300-304.
【5】GB/T 23212-2008牛奶和奶粉中黄曲霉毒素B1、B2、G1、G2、M1、M2的测定 液相色谱-荧光检测法[S].
【6】SN/T 1664-2005牛奶和奶粉中黄曲霉毒素M1、B1、B2、G1、G2含量的测定[S].
【7】BELTRN E,IBANEZ M,SANCHO J V,et al.UHPLC-MS/MS highly sensitive determination of aflatoxins,the aflatoxin metabolite M1 and ochratoxin A in baby food and milk[J].Food Chemistry,2011,126:737-744.
【8】董彬,杨立新,李斌,等.多功能柱净化液相色谱-质谱-质谱法测定牛奶中黄曲霉毒素M1[J].现代农药,2011,10(4):38-40.
【9】GB/T 22992-2008牛奶和奶粉中玉米赤霉醇、玉米赤霉酮、己烯雌酚、己烷雌酚、双烯雌酚残留量的测定液相色谱-串联质谱法[S].
【10】卢安根,莫建光,杜寒春,等.酶联免疫法快速检测牛奶及其制品中的黄曲霉毒素B1[J].广西科学院学报,2010,26(3):306-308.
【11】NY/T 1664-2008牛乳中黄曲霉毒素M1的快速检测双流向酶联免疫法[S].
【12】闫磊,李卓,张燕.牛奶中黄曲霉毒素的放射免疫法检测[J].食品研究与开发,2010,31(1):135-137.
【13】李佐卿,章再婷,谢东华,等.免疫亲和柱高效液相色谱法快速测定牛奶和奶粉中黄曲霉毒素M1、B1、B2、G1、G2[J].理化检验-化学分册,2005,42(6):406-408.
【2】GB 2761-2011食品中真菌毒素限量[S].
【3】Commission Regulation (EC) No 1881/2006Setting maximum levels for certain contaminants in foodstuffs[S].
【4】陈瑞春,段文仲,吕红英,等.免疫亲和层析净化-高效液相色谱法同时测定牛奶和奶粉中黄曲霉毒素B1、B2、G1、G2、M1、M2[J].食品科技,2011,36(8):300-304.
【5】GB/T 23212-2008牛奶和奶粉中黄曲霉毒素B1、B2、G1、G2、M1、M2的测定 液相色谱-荧光检测法[S].
【6】SN/T 1664-2005牛奶和奶粉中黄曲霉毒素M1、B1、B2、G1、G2含量的测定[S].
【7】BELTRN E,IBANEZ M,SANCHO J V,et al.UHPLC-MS/MS highly sensitive determination of aflatoxins,the aflatoxin metabolite M1 and ochratoxin A in baby food and milk[J].Food Chemistry,2011,126:737-744.
【8】董彬,杨立新,李斌,等.多功能柱净化液相色谱-质谱-质谱法测定牛奶中黄曲霉毒素M1[J].现代农药,2011,10(4):38-40.
【9】GB/T 22992-2008牛奶和奶粉中玉米赤霉醇、玉米赤霉酮、己烯雌酚、己烷雌酚、双烯雌酚残留量的测定液相色谱-串联质谱法[S].
【10】卢安根,莫建光,杜寒春,等.酶联免疫法快速检测牛奶及其制品中的黄曲霉毒素B1[J].广西科学院学报,2010,26(3):306-308.
【11】NY/T 1664-2008牛乳中黄曲霉毒素M1的快速检测双流向酶联免疫法[S].
【12】闫磊,李卓,张燕.牛奶中黄曲霉毒素的放射免疫法检测[J].食品研究与开发,2010,31(1):135-137.
【13】李佐卿,章再婷,谢东华,等.免疫亲和柱高效液相色谱法快速测定牛奶和奶粉中黄曲霉毒素M1、B1、B2、G1、G2[J].理化检验-化学分册,2005,42(6):406-408.
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