色谱

色谱 ›› 2017, Vol. 35 ›› Issue (8): 808-815.DOI: 10.3724/SP.J.1123.2017.03035

• 研究论文 • 上一篇    下一篇

超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定焙烤食品及其原料中11种真菌毒素

李蓉1, 何春梅1,2, 杨璐齐1,2, 王勇1, 张朋杰1, 高永清2   

  1. 1. 中山出入境检验检疫局, 广东 中山 528400;
    2. 广东药科大学食品科学学院, 广东 中山 528458
  • 收稿日期:2017-03-27 出版日期:2017-08-08 发布日期:2013-11-25
  • 通讯作者: 李蓉,Tel:88830078,E-mail:lirong828@126.com;高永清,Tel:88207955,E-mail:yongqingg@163.com
  • 基金资助:

    广东省省级科技计划项目（2014A040401011）；国家质检总局科技计划项目（2015IK260）；中山市社会公益重大专项（2015B2295）.

Determination of 11 mycotoxins in baked foods and raw materials by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry

LI Rong1, HE Chunmei1,2, YANG Luqi1,2, WANG Yong1, ZHANG Pengjie1, GAO Yongqing2   

  1. 1. Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528400, China;
    2. Guangdong Pharmaceutical University, Zhongshan 528458, China
  • Received:2017-03-27 Online:2017-08-08 Published:2013-11-25
  • Supported by:

    Science and Technology Planning Project of Guangdong Province of China (No. 2014A040401011); Science and Technology Planning Project of General Administration of Quality Supervision Inspection and Quarantine of the People's Republic of China (No. 2015IK260); Social Public Welfare Major Project of Zhongshan City (No. 2015B2295).

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摘要：

建立了超高效液相色谱-四极杆/静电场轨道阱高分辨质谱（UPLC-HRMS）测定焙烤食品及其原料中11种真菌毒素的检测分析方法。样品经20 mL含1%（体积分数）甲酸的乙腈-水（9：1，v/v）溶液提取，经2.0 g无水硫酸、0.5 g氯化钠和300 mg C18盐析、净化后进行检测。采用CORTECS C18色谱柱（100 mm×2.1 mm，1.6 μ m），以含0.1%（体积分数）甲酸的2 mmol/L乙酸铵溶液和含0.1%（体积分数）甲酸的2 mmol/L乙酸铵甲醇溶液为流动相进行梯度洗脱。结果显示，11种真菌毒素在各自的质量浓度范围内线性关系良好（相关系数r2≥0.9960），方法的定量限为0.15~20.00 μ g/kg，样品加标回收率为64.38%~122.61%，相对标准偏差为1.52%~12.99%（n=6）。该方法简单快速、灵敏度高、结果准确、可靠，利用该方法可有效测定焙烤食品及其原料中常见真菌毒素的含量。

关键词: 焙烤食品, 超高效液相色谱-高分辨质谱, 真菌毒素

Abstract:

A method for the determination of 11 mycotoxins in baked foods and raw materials by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry (UPLC-HRMS) is reported in this paper. The samples were extracted with 20 mL 90% (v/v) acetonitrile aqueous solution containing 1% (v/v) formic acid, and the extracts were salted out by 2.0 g MgSO4 and 0.5 g NaCl, cleaned up by 300 mg C18. The analytes were carried out on a CORTECS C18 column (100 mm×2.1 mm, 1.6 μ m) by gradient elution with 2 mmol/L ammonium acetate with 0.1% (v/v) formic acid aqueous solution and 2 mmol/L ammonium acetate methanol with 0.1% (v/v) formic acid. The results showed that the 11 mycotoxins had good linear relationships in their respective mass concentration ranges. The correlation coefficients were not less than 0.9960 and the limits of quantitation (LOQs) were from 0.15 to 20.00 μ g/kg. The recoveries of the 11 mycotoxins in bread ranged from 64.38% to 122.61% with the relative standard deviations (RSDs) from 1.52% to 12.99% at three spiked levels (n=6). The method is demonstrated to be simple, fast, highly sensitive, reliable and it is effective to detect common mycotoxins in baked foods and raw materials.

Key words: baked foods, mycotoxins, ultra-high performance liquid chromatography-high-resolution mass spectrometry (UPLC-HRMS)

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