摘要
建立利用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱联用技术同时测定乳及乳制品中21种真菌毒素的方法。乳及乳制品经酸化乙腈提取后,采用Captiva-EMR Lipid净化柱净化,以C18色谱柱进行色谱分离,质谱采用全扫描/数据依赖的二级扫描模式(full scan data-dependent MS/MS acquisition mode,FullMS/ddMS2)分别在正、负离子模式下检测,外标法定量。21种真菌毒素在一定浓度范围内均具有良好的线性关系,相关系数(r)均大于0.99,定量限范围为1.0~93.8μg/kg,在三个加标水平下,平均回收率为60.3%~107.0%,相对标准偏差(RSD)为0.4%~14.4%。应用本方法对市售粉状和液态乳及乳制品进行检测,一个水果添加酸奶样品检出黄曲霉毒素B2。该方法快速、准确,适用于乳及乳制品中多真菌毒素的快速测定,并可用于真菌毒素风险的高效筛查。
A method for the simultaneous determination of 21 mycotoxins in milk and dairy products using ultra performance liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometry technology was established.After the milk and dairy products were extracted with acidified acetonitrile, they were purified by a Captiva-EMR Lipid purification column and chromatographically separated by a C18 column. The mass spectrometry adopt full scan datadependent MS/MS acquisition mode(Full MS/ddMS2) detected in positive and negative ion modes, and quantified by external standard method. The 21 mycotoxins all had a good linear relationship within a certain concentration range, the correlation coefficients(r) were greater than 0.99, the limits of quantification were 1.0~93.8 μg/kg, and the average recoveries of all mycotoxins were 60.3%~107.0% at three different levels, and the relative standard deviations(RSD)ranged between 0.4%~14.4%. This method was used to detect commercially available powdered and liquid milk and dairy products. Aflatoxin B2 was detected in a fruit-added yogurt sample. The method was fast, accurate, suitable for the rapid determination of multiple mycotoxins in milk and dairy products, which could be used for efficient screening of mycotoxins risks.
作者
何卓霖
穆蕾
王涛
王亮
谢云峰
HE Zhuolin;MU Lei;WANG Tao;WANG Liang;XIE Yunfeng(College of Life Science and Technology,Xinjiang University,Urmuqi 830046,China;Beijing Key Laboratory of Nutrition Health and Food Safety,COFCO Nutrition&Health Research Institute,Beijing 102209,China)
出处
《食品工业科技》
CAS
北大核心
2022年第6期302-310,共9页
Science and Technology of Food Industry
基金
“十三五”国家重点研发计划项目(2017YFC1601603)。
关键词
乳及乳制品
真菌毒素
超高效液相色谱-四极杆/静电场轨道阱高分辨质谱
风险监测
milk and dairy products
mycotoxins
ultra performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry
risk monitoring
