食品科学 ›› 2009, Vol. 30 ›› Issue (4): 162-165.doi: 10.7506/spkx1002-6630-200904032

• 分析检测 • 上一篇    下一篇

高效液相色谱- 电喷雾三级四极杆质谱测定苹果、山楂、番茄制品中棒曲霉素的研究

杨冀州1,魏 蔚1,祝伟霞1,2,刘亚风1   

  1. 1.河南出入境检验检疫局 2.郑州大学化学系
  • 收稿日期:2008-02-25 修回日期:2008-06-03 出版日期:2009-02-15 发布日期:2010-12-29
  • 通讯作者: 杨冀州 E-mail:jzyang@163.com
  • 基金资助:

    国家认证认可监督管理委员会资助项目(2006B384x)

High Performance Liquid Chromatography Tandem Mass Spectrometry Method for Determination of Patulin in Apple, Hawthorn and Tomato Products

YANG Ji-zhou1,WEI Wei1,ZHU Wei-xia1,2,LIU Ya-feng1   

  1. (1. Henan Entry - Exit Inspection and Quarantine Bureau, Zhengzhou 450003, China;
    2. Department of Chemistry, Zhengzhou University, Zhengzhou 450001, China)
  • Received:2008-02-25 Revised:2008-06-03 Online:2009-02-15 Published:2010-12-29
  • Contact: YANG Ji-zhou1 E-mail:jzyang@163.com

摘要:

建立了苹果、山楂、番茄制品中棒曲霉素总量的提取方法和液相色谱串联质谱确证方法。清汁样品用乙腈稀释后直接过MycoSep 228 真菌霉素多功能净化柱;浊汁、固体样品用果胶酶水解后,再用乙酸乙酯提取样品中棒曲霉素,浓缩后经MycoSep 228 柱净化,用Atlantis dC18 色谱柱分离,液相色谱串联质谱测定,电喷雾负离子(ESI -)多反应模式下监测;实验结果表明,样品中棒曲霉素浓度在1.0~200μg/kg 范围内时与其峰面积成良好线性关系,检测低限为2.0μg/kg,3 个加标水平下回收率为76.0%~95.3%,相对标准偏差为5.4%~11.2%。该方法选择性好,灵敏度高,定性可靠,可满足苹果、山楂、番茄制品中棒曲霉素测定的要求。

关键词: 棒曲霉素, 液相色谱-质谱/质谱, 电喷雾, 真菌毒素多功能净化柱, 苹果制品, 山楂制品, 番茄制品

Abstract:

A method was developed to clean-up and detect total patulin in of apple, hawthorn and tomato products using HPLCMS/ MS. Clear juice was diluted directly with acetonitrile and cleaned-up with MycoSep 228 multifunctional clean-up column. Cloudy juice or solid samples were pre-treated with pectinase, extracted with acetate ethyl, and then cleaned-up with MycoSep 228. Chromatographic separation was performed on a column Atlantis dC18 and determination was achieved by HPLC-MS/MS with ESI-(electronic spray ionization). The results demonstrated that the linear ranges are from 1.0 μg/kg to 200 μg/kg with the detection limit of 2.0 μg/kg. The average recoveries and the relative standard deviations range 76.0% to 95.3% and 5.4% to 11.2%. The method is simple, rapid, accurate and suitable for the quantification and confirmation determination of patulin in apples, hawthorn, tomato products.

Key words: patulin, HPLC-MS/MS, ESI, mycotoxin multifunctional clean-up column, apple products, hawthorn products, tomato products

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