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基于UPLC-MS-MS技术定量确证小麦中10种真菌毒素

Quantitative Determination of 10 Kinds of Mycotoxins in Wheat by UPLC-MS-MS

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【作者】 孟繁磊牛红红何智勇张振都蔡红梅宋志峰

【Author】 Meng Fan-lei;Niu Hong-hong;He Zhi-yong;Zhang Zhen-du;Cai Hong-mei;Song Zhi-feng;Institute of Agricultural Quality Standard and Testing Testing Technology,Jilin Academy of Agricultural Sciences,Laboratory of Quality and Safety Risk Asessment for Agro-products(Changchun),Ministry of Agriculture;

【机构】 吉林省农业科学院农业质量标准与检测技术研究所农业部农产品质量安全风险评估实验室

【摘要】 建立了小麦中黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、脱氧雪腐镰刀菌烯醇、雪腐镰刀菌烯醇、3-乙酰脱氧雪腐镰刀菌烯醇、脱氧雪腐镰刀菌烯醇-3-葡萄糖苷、15-乙酰脱氧雪腐镰刀菌烯醇和玉米赤霉烯酮等10种真菌毒素的超高液相色谱-三重四级杆串联质谱法检测的方法。小麦样品经乙腈-水-乙酸溶液震荡超声提取后,采用多功能净化柱净化。待测物经Kinetex SB-C18色谱柱分离,甲醇-0.1%甲酸为流动相,梯度洗脱,正负模式同时扫描,三重串联四级杆质谱多反应离子监测(MRM)方式检测,基质标准校正,外标法定量。结果表明,在一定的浓度范围内,10种真菌毒素线性关系良好,相关系数均大于0.999,方法的检出限为0.0151μg/kg,空白样品中添加高中低不同浓度的真菌毒素的回收率为65.12%89.16%,RSD%(n=6)在4.26%9.46%之间。该方法分析速度快、重复性好、灵敏度高,适合小麦中多种真菌毒素的高灵敏度快速测定。

【Abstract】 A method for the quantitative determination of 10 mycotoxins, such as aflatoxin B1, aflatoxin B2, aflatoxin G1,aflatoxin G2, deoxynivalenol, 3-deoxynivalenol, 3-acetyl deoxynivalenol, 15-acetyl deoxynivalenol and zearalenone in wheat by ultra-high liquid chromatography triple quadrupole tandem mass spectrometry was developed. Wheat samples were extracted by ultrasonic with acetonitrile-water-acetic acid solution, and purified by multi-functional purification column. Chromatographic analysis was carried out in a Kinetex SB-C18 column, the binary mobile phase consisted of methanol and 0.1% formic acid, and the system was run with a gradient program. Mass spectrometric detection was carried out on Xevo TQ mass spectrometer with negative and positive ionization mode. Quantification analysis was performed in multiple reaction monitoring(MRM), matrix standard calibration, and external standard method quantitative. The results demonstrated that the 10 mycotoxins had good linear relationship and the correlation coefficients were more than 0.999. The detection limit(LOD) of the method was 0.015-1 μg/kg, the average recoveries in the blank matrix ranged from 65.12% to 89.16% with relative standard deviation(RSD, n=6) of 4.26%-9.46%. The method in this study was fast analysis, good reproducibility and high sensitivity, it is suitable for rapid determination of various fungal toxins in wheat.

【基金】 农业部/国家农产品质量安全风险评估重大专项中课题(GJFP201600001003)
  • 【分类号】O657.63;TS210.7
  • 【被引频次】10
  • 【下载频次】213
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