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食品研究与开发:2016,37(3):156-160
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液相色谱-串联质谱测定小麦粉中 11种真菌毒素
李磊1,李海畅2,周贻兵1,林野1
(1. 贵州省疾病预防控制中心,贵州 贵阳 550004;2. 贵阳市疾病预防控制中心,贵州 贵阳 550002)
Determination of 11 Mycotoxins in Wheat Flour by Performance Liquid Chromatography-tandem Mass Spectrometry
LI Lei1, LI Hai-chang2, ZHOU Yi-bing1, LIN Ye1
(1. Guizhou Provincial Physical and Chemical Inspection of Center for Disease Control and Prevention, Guiyang 550004, Guizhou, China; 2. Guiyang Provincial Center for Disease Control and Prevention, Guiyang 550002,Guizhou, China)
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投稿时间:2015-11-15    
中文摘要: 建立小麦粉中 11 种真菌毒素的超高效液相色谱-串联质谱检测方法。样品用乙腈-水溶液提取,经多功能净化 柱 PriboFast 100 进行净化,采用 XTerra MS C18 色谱柱进行分离,以 20 mmol/L 乙酸铵溶液和乙腈梯度洗脱,利用超高 效液相色谱-串联质谱进行分析。11 种真菌毒素在测定浓度范围内线性关系良好,各组分相关系数 R2 >0.998,加标回收 率范围 72.4 %~90.7 %,方法精密度范围 6.2 %~11.8 %,测定各组分真菌毒素定量限范围 1.2 μg/kg~2.0 μg/kg。该方法前处 理过程简洁、灵敏度高、重现性好,适用于小麦粉中 11 种真菌毒素的测定。
Abstract:Objects Establish method to detect the 11 kinds of mycotoxins in wheat flour by ultra performance liquid chromatography - tandem mass spectrometry. Methods Samples were crushed and sieved extracted by aqueous acetonitrile, purified by multifunctional cleaning column PriboFast 100, separated by Xterra MS C18 chromatographic column, gradient eluted by 20 mmol/L ammonium acetate and acetonitrile, and detected by ultra high performance liquid chromatography- tandem mass spectrometry. Results The 11 kinds of mycotoxins show good linear relationship between the concentration range, components correlation coefficient R2>0.998, standard addition recovery range of 72.4 %-90.7 % , precision range 6.2 %-11.8 % , and LOQ components range 1.2 μg/kg -2.0 μg/kg. Conclusion The method shows high sensitivity, accurate, reproducible, which suitable for detection of 11 kinds of mycotoxins in wheat flour.
文章编号:201603040     中图分类号:    文献标志码:A
基金项目:国家自然科学基金(21346008);河北省自然科学基金(B2011202056)
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