复合免疫亲和柱净化-超高效液相色谱-串联质谱法同时测定鲜奶中赭曲霉毒素A等毒素  

Simultaneous determination of ochratoxin A and other toxins in fresh milk by composite immunoaffinity column purification-ultra performance liquid chromatography tandem mass spectrometry

作　　者：武茂瑞 刘利亚 林野[2] 周贻兵[2] 吴玉田[2] 孟春杨 WU Maorui;LIU Liya;LIN Ye;ZHOU Yibing;WU Yutian;MENG Chunyang(School of Public Health and Health Management,Guizhou Medical University,Key Laboratory of Environmental Pollution and Disease Control by Ministry of Education,Guiyang 561113,China;Guizhou Provincial Center for Disease Control and Prevention,Guiyang 550004,China)

机构地区：[1]贵州医科大学公共卫生与健康学院环境污染与疾病监控教育部重点实验室,贵阳561113 [2]贵州省疾病预防控制中心,贵阳550004

出　　处：《化学分析计量》2025年第2期77-83,共7页Chemical Analysis And Meterage

摘　　要：建立复合免疫亲和柱净化-同位素内标-超高效液相色谱-串联质谱法同时测定鲜奶中赭曲霉毒素A和6种玉米赤霉烯酮类毒素。样品添加内标后,经过混匀离心和过滤除脂,进行免疫亲和柱净化后,在C_(18)柱上分离,以0.1%(体积分数)甲酸水-甲醇为流动相梯度洗脱,电离源负离子模式扫描,多反应监测模式定量。在质量浓度为0.2~9.0 ng/m L内,7种真菌毒素的质量浓度与对应的色谱峰面积均表现出良好的线性关系,相关系数均大于0.999。7种真菌毒素的回收率为80.4%~109.2%,测试结果的相对标准偏差为1.3%~10.4%(n=6)。赭曲霉毒素A的检出限和定量限分别为0.000 3、0.001μg/kg,6种玉米赤霉烯酮类毒素的检出限和定量限分别为0.003、0.01μg/kg。该方法精确可靠,适用于牛奶中赭曲霉毒素A和6种玉米赤霉烯酮类毒素的同时检测。A method for the simultaneous determination of ochratoxin A and six zearalenones in fresh milk by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)with isotope internal standard after purification by composite immunoaffinity column was established.After the internal standard was added to the sample,it was centrifuged and filtered to remove fat.After purification by immunoaffinity column,it was separated on a C18 column with 0.1%(volume fraction)formic acid water-methanol as the mobile phase for gradient elution.The ion source was scanned in negative ion mode and quantified in multiple reaction monitoring mode.The results showed that there was a good linear relationship between the mass concentration of 7 mycotoxins and the corresponding chromatographic peak area in the mass concentration range of 0.2-9.0 ng/mL,and the correlation coefficient was greater than 0.999.The recoveries of 7 mycotoxins were 80.4%-109.2%,and the relative standard deviations of phase test results were 1.3%-10.4%.The limits of detection and limits of quantitation of ochratoxin A were 0.0003 and 0.001μg/kg,respectively.The limit of detection and limit of quantitation of six zearalenones were 0.003 and 0.01μg/kg,respectively.The method is accurate and reliable,and is suitable for the simultaneous detection of ochratoxin A and six zearalenone toxins in milk.

关 键 词：免疫亲和柱 同位素内标 超高效液相色谱-串联质谱 鲜奶 玉米赤霉烯酮类毒素 赭曲霉毒素A 

分 类 号：O657[理学—分析化学]