湖北农业科学 ›› 2024, Vol. 63 ›› Issue (6): 187-192.doi: 10.14088/j.cnki.issn0439-8114.2024.06.030

• 检测分析 • 上一篇    下一篇

超高效液相色谱-四级杆飞行时间质谱测定三七中九种真菌毒素

程龙1, 李云飞2, 吴思超3, 赵风情2, 张国帅2, 何友艳2, 陶蕾2, 王英2   

  1. 1.云南农业大学食品科学技术学院,昆明 650201;
    2.昆明海关技术中心,昆明 650208;
    3.黄埔海关技术中心,广东 东莞 523071
  • 收稿日期:2022-11-17 出版日期:2024-06-25 发布日期:2024-06-26
  • 通讯作者: 王 英(1985-),女,云南大理人,工程师,博士,主要从事食品药品安全研究,(电话)15925205086(电子信箱)594916964@qq.com。
  • 作者简介:程 龙(1991-),男,安徽安庆人,在读硕士研究生,研究方向为食品加工与安全,(电话)13759498239(电子信箱)934042353@qq.com。
  • 基金资助:
    海关总署科研项目(2021HK208); 林下中药材产品质量管控数据化关键技术研究项目(202102AE090042)

Determination of nine mycotoxins in Panax notoginseng by ultra high performance liquid chromatography quadrupole time-of-flight mass spectrometry

CHENG Long1, LI Yun-fei2, WU Si-chao3, ZHAO Feng-qing2, ZHANG Guo-shuai2, HE You-yan2, TAO Lei2, WANG Ying2   

  1. 1. College of Food Science and Technology, Yunnan Agricultural University, Kunming 650201, China;
    2. Technology Center of Kunming Customs, Kunming 650208, China;
    3. Technology Center of Huangpu Customs, Dongguan 523071, Guangdong, China
  • Received:2022-11-17 Published:2024-06-25 Online:2024-06-26

摘要: 建立一种三七中9种真菌毒素的超高效液相色谱-四极杆飞行时间质谱筛查与确证方法,快速筛查三七中9种真菌毒素(黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、伏马菌素B1、伏马菌素B2、脱氧雪腐镰刀菌烯醇、玉米赤霉烯酮、赭曲霉毒素A)的残留量。色谱柱为Phenomenex Kinetex C18(100 mm×2.1 mm,2.6 μm),以0.1%甲酸水溶液和0.1%甲酸甲醇水溶液为流动相进行梯度洗脱,正离子扫描,基质匹配外标法定量。结果表明,9种真菌毒素分别在0.1~100.0、5.0~1 000.0、0.5~500.0 μg/L 浓度范围内具有良好的线性关系,相关系数均大于0.990 00,方法定量限为0.3~15.0 μg/kg,在高、中、低3个浓度加标水平下,回收率为71.22%~98.57%,相对标准偏差为2.31%~ 6.72%。该方法在没有对照品的情况下,可与质谱数据库中一级、二级质谱的精确质量数和碎片离子信息等进行匹配,降低了试验成本,具有简便、快速、高效、准确等优点,适用于三七中真菌毒素残留的快速筛查和测定。

关键词: 超高效液相色谱-四级杆飞行时间质谱, 三七, 真菌毒素

Abstract: An ultra high performance liquid chromatography quadrupole time-of-flight mass spectrometry screening and confirmation method was established for 9 types of mycotoxins in Panax notoginseng. The residual levels of 9 types of mycotoxins (Aflatoxin B1、Aflatoxin B2、Aflatoxin G1、Aflatoxin G2、Fumonitoxin B1、Fumonitoxin B2、Deoxynivalenol、Zearalenone、Ochratoxin A) in Panax notoginseng were quickly screened. The chromatographic column was Phenomenex Kinetex C18 (100 mm × 2.1 mm, 2.6 μm), and gradient elution was performed using 0.1% formic acid aqueous solution and 0.1% formic acid methanol solution as mobile phases. Positive ion scanning and the matrix matching external standard method were used for quantification. The results showed that 9 types of mycotoxins had good linear relationships within the concentration ranges of 0.1~100.0, 5.0~1 000.0, and 0.5~500.0 μg/L, respectively,the correlation coefficients were all greater than 0.990 00, and the quantitative limit of the method was 0.3~15.0 μg/kg. At three spiked levels of high, medium, and low concentrations, the recovery rate was 71.22%~98.57%, and the relative standard deviation was 2.31%~6.72%. This method could match the precise mass numbers and fragment ion information of primary and secondary mass spectra in the mass spectrometry database without reference materials, reducing experimental costs. It had the advantages of simplicity, rapidness, efficiency, and accuracy, and was suitable for the rapid screening and determination of mycotoxins residues in Panax notoginseng.

Key words: ultra high performance liquid chromatography quadrupole time-of-flight mass spectrometry, Panax notoginseng, mycotoxins

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