职业与健康 ›› 2024, Vol. 40 ›› Issue (23): 3194-3199.

• 论著 • 上一篇    下一篇

小麦粉中4种交链孢霉毒素的固相萃取-高效液相色谱-串联质谱测定法

肖潇, 王庆国, 何川川, 祖力乎马尔·艾海提, 田家磊, 李方   

  1. 新疆维吾尔自治区疾病预防控制中心理化所,新疆 乌鲁木齐 830002
  • 收稿日期:2024-04-07 修回日期:2024-05-07 出版日期:2024-12-01 发布日期:2026-04-09
  • 通信作者: 李方,副主任医师,E-mail:115144679@qq.com
  • 作者简介:肖潇,女,高级实验师,主要从事食品理化检测工作。
  • 基金资助:
    新疆维吾尔自治区自然科学基金(2020D01C083)

Determination of four Alternaria toxin in wheat flour by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

XIAO Xiao, WANG Qingguo, HE Chuanchuan, Zulihumaer Aihaiti, TIAN Jialei, LI Fang   

  1. Institute of Physics and Chemistry,Xinjiang Uygur Autonomous Region Center for Disease Control and Prevention,Urumqi,Xinjiang 830002,China
  • Received:2024-04-07 Revised:2024-05-07 Online:2024-12-01 Published:2026-04-09
  • Contact: LI Fang,Associate chief physician,E-mail:115144679@qq.com

摘要: 目的 建立一种固相萃取-高效液相色谱-串联质谱法测定小麦粉中4种交链孢霉毒素。方法 样品用乙腈-0.05 mol/L磷酸二氢钠(50/50)溶液提取,HLB固相萃取柱净化,以甲醇-1 mmol/L碳酸氢铵水溶液为流动相,梯度模式洗脱,经HSS T3色谱柱分离,三种四级杆质谱检测,内标法定量。结果 4种交链孢霉毒素在0.2~50 ng/mL线性范围内回归方程线性关系良好,相关系数r>0.998,加标回收率为76.2%~110.6%,相对标准偏差为4.04%~8.74%,检出限在0.02~0.75 μg/kg,定量限在0.06~2.50 μg/kg。结论 该方法灵敏度高、准确性好,检出限、加标回收率和精密度满足方法学的要求,适用于小麦粉中4种交链孢霉毒素的测定。

关键词: 交链孢霉毒素, 小麦粉, 高效液相色谱串联质谱, 固相萃取

Abstract: Objective To establish a solid phase extraction-high performance liquid chromatography-tandem mass spectrometry method for the determination of four types of Alternaria toxins in wheat flour. Methods The samples were extracted with acetonitrile-0.05 mol/L ammonium dihydrogen phosphate(50/50),purified by HLB solid-phase extraction column,and eluted in gradient procedure using methanol-1 mmol/L ammonium bicarbonate aqueous solution as the mobile phase,separated by HSS T3 chromatography column,detected by three quadrupole mass spectrometry,and quantified by internal standard method. Results The regression equation of the four types of Alternaria toxins showed a good linear relationship within the range of 0.2-50 ng/mL,with a correlation coefficient r>0.998. The recoveries ranged from 76.2% to 110.6%,the relative standard deviation(RSD) was 4.04%-8.74%,the detection limit was 0.02-0.75 μg/kg,and the quantification limit was 0.06-2.50 μg/kg. Conclusion This method has high sensitivity,good accuracy,detection limit,recovery and precision that meet the requirements of methodology. It is suitable for the determination of four types of Alternaria toxins in wheat flour.

Key words: Alteration toxin, Wheat flour, High performance liquid chromatography-tandem mass spectrometry, Solid phase extraction

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