色谱

色谱 ›› 2018, Vol. 36 ›› Issue (6): 566-572.DOI: 10.3724/SP.J.1123.2018.02008

• 技术与应用 • 上一篇    下一篇

免疫亲和固相萃取-超高效合相色谱-串联质谱法同时测定牛奶中6种玉米赤霉醇类化合物残留

章璐幸, 孙洁胤, 王延辉, 吴惠芳, 俞松林   

  1. 浙江医药高等专科学校, 宁波, 315100
  • 收稿日期:2018-02-09 出版日期:2018-06-08 发布日期:2014-04-24
  • 通讯作者: 俞松林,E-mail:2290140894@qq.com
  • 基金资助:

    宁波市社发攻关项目（2014C50076）；浙江省食品药品监督管理系统科技计划项目（SP201609）.

Simultaneous determination of six zeranols in milk samples by immunoaffinity solid phase extraction coupled with ultra-performance convergence chromatography-tandem mass spectrometry

ZHANG Luxing, SUN Jieyin, WANG Yanhui, WU Huifang, YU Songlin   

  1. Zhejiang Pharmaceutical College, Ningbo 315100, China
  • Received:2018-02-09 Online:2018-06-08 Published:2014-04-24
  • Supported by:

    Social Development Project of Ningbo (No.2014C50076);Zhejiang Food and Drug Supervision System Science and Technology Project (No.SP201609).

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被引次数

1

摘要：

建立了免疫亲和固相萃取（IAC-SPE）-超高效合相色谱-串联质谱（UPC2-MS/MS）同时测定牛奶中α-玉米赤霉醇、β-玉米赤霉醇、α-玉米赤霉烯醇、β-玉米赤霉烯醇、玉米赤霉烯酮和玉米赤霉酮残留的分析方法。样品用去离子水稀释，经IAC-SPE富集净化后，采用Waters ACQUITY UPC2 Torus 2-PIC色谱柱（50 mm×3.0 mm，1.7 μm）分离，以超临界CO2和0.1%（v/v）甲酸甲醇溶液为流动相，经梯度洗脱后在ESI-模式下检测。经过稀释离心的牛奶样品采用免疫亲和柱净化后没有明显的基质效应，6种目标化合物在1~200 ng/mL范围内线性关系良好，相关系数（r2）≥0.9957；6种目标化合物在3个加标水平下的平均回收率为75.9%~106.5%，日内和日间精密度均≤11.4%。该法专属性好，操作简便，有机溶剂使用量小，与已有的样品测定方法比较更绿色环保，可用于牛奶中α-玉米赤霉醇、β-玉米赤霉醇、α-玉米赤霉烯醇、β-玉米赤霉烯醇、玉米赤霉酮和玉米赤霉烯酮的残留检测。

关键词: 超高效合相-串联质谱, 固相萃取, 免疫亲和柱, 牛奶, 玉米赤霉醇类化合物

Abstract:

A method was developed for the simultaneous determination of α-zearalanol, β-zearalanol, α-zearalenol, β-zearalenol, zearalenone and zearalanone residues in milk samples by ultra-performance convergence chromatography-tandem mass spectrometry (UPC2-MS/MS) after immunoaffinity column-solid phase extraction (IAC-SPE). The sample was diluted with deionized water and cleaned with IAC-SPE. The chromatographic separation was performed on an ACQUITY UPC2 Torus 2-PIC column (50 mm×3.0 mm, 1.7 μm) using the mobile phases of supercritical carbon dioxide and methanol containing 0.1% (v/v) formic acid with gradient elution. The separated compounds were detected in negative electrospray ionization (ESI-) mode. The results showed no significant matrix effect after cleaning by IAC-SPE. The calibration curves of the six compounds were linear in the range of 1-200 ng/mL (correlation coefficients (r2) ≥ 0.9957). The recoveries were 75.9%-106.5% in the three spiked levels, and the intra-day and inter-day precisions were no more than 11.4%. The method is specific, environment friendly, and is suitable for the rapid determination of α-zearalanol, β-zearalanol, α-zearalenol, β-zearalenol, zearalenone and zearalanone residues in milk samples.

Key words: immunoaffinity column (IAC), milk, solid phase extraction (SPE), ultra-performance convergence chromatography-tandem spectrometry (UPC2-MS/MS), zeranols

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