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当前位置: 首页 > 文章 > 固相萃取柱净化-超高效液相色谱-串联质谱法快速测定液态乳中14种真菌毒素 食品科学 2018 (18) 292-301
Position: Home > Articles > Determination of 14 Mycotoxins in Liquid Milk by Solid-Phase Extraction Coupled with Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry FOOD SCIENCE 2018 (18) 292-301

固相萃取柱净化-超高效液相色谱-串联质谱法快速测定液态乳中14种真菌毒素

作  者：
孙晓冬;郝杰;毛婷;邵瑞婷;姜洁
单  位：
北京市食品安全监控和风险评估中心
关键词：
液态乳;固相萃取柱;超高效液相色谱-串联质谱;真菌毒素;快速
摘  要：
建立使用固相萃取柱净化液态乳中14种真菌毒素(黄曲霉毒素B_1、黄曲霉毒素B_2、黄曲霉毒素G_1、黄曲霉毒素G_2、黄曲霉毒素M_1、赭曲霉毒素A、橘霉素、T-2毒素、杂色曲霉素、伏马毒素B_1、伏马毒素B_2、玉米赤霉烯酮、脱氧雪腐镰刀菌烯醇、青霉酸)多残留的超高效液相色谱-串联质谱检测方法。样品经含0.1%甲酸-乙腈沉淀蛋白和提取,固相萃取柱Oasis PRi ME HLB净化后,以0.1%甲酸溶液与乙腈为流动相,经ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm)分离,梯度洗脱,采用电喷雾-正离子多反应监测模式,外标法定量。结果表明:14种真菌毒素的定量限(R_(SN)≥10)为0.5~5μg/kg,高、中、低3个添加水平时,平均回收率为67.7%~112.7%,相对标准偏差为0.43%~7.28%。该方法的检测速度快,净化效果较好,基质干扰较少,灵敏度高,结果准确、可靠,可用于液态乳中真菌毒素的检测分析。
译  名：
Determination of 14 Mycotoxins in Liquid Milk by Solid-Phase Extraction Coupled with Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry
作  者：
SUN Xiaodong;HAO Jie;MAO Ting;SHAO Ruiting;JIANG Jie;Beijing Municipal Center for Food Safety Monitoring and Risk Assessment;
关键词：
liquid milk;;solid-phase extraction column;;ultra-performance liquid chromatography-tandem mass spectrometry;;mycotoxins;;rapid detection
摘  要：
A rapid method was established for detecting 14 mycotoxins(aflatoxin B_1, aflatoxin B_2, aflatoxin G_1, aflatoxin G_2, aflatoxin M_1, ochratoxin A, citrinin, T-2 toxin, sterigmatocystin, fumonisin B_1, fumonisin B_2, zearalenone, deoxynivalenol, and penicillic acid) in liquid milk by solid-phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Samples were defatted and extracted with 0.1% formic acid acetonitrile and the extract was cleaned up with Oasis PRi ME HLB solid-phase extraction column. The analytes were separated on HSS T3 column(2.1 mm × 100 mm, 1.8 μm) with a mobile phase composed of 0.1% formic acid and acetonitrile using gradient elution. Detection was carried out by tandem mass spectrometry using positive ionization in the multiple-reaction monitoring(MRM) mode. An external standard method was applied for quantification. Results showed that the limits of quantitation(LOQs) of 14 mycotoxins in matrices were between 0.5 and 5 μg/kg. Average recoveries at 3 different spiked levels were 67.7%–112.7% with relative standard deviation(RSD) of 0.43%–7.28%. With the advantages of rapidity, high purification efficiency, low matrix interference and accurate and reliable results, the method is useful for the analysis of mycotoxins in liquid milk.

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