超高效液相色谱-三重四极杆串联质谱技术快速检测酵米面中米酵菌酸和毒黄素的含量  

Rapid determination of bongkrekic acid and toxoflavin in ferment corn flour by ultra-performance liquid chromatography-triple quadrupole tandem mass spectrometry

作　　者：张伟[1] 谭洁冰 冯光伟 马青青[1] 苏永恒[1] 张榕杰[1] ZHANG Wei;TAN Jie-bing;FENG Guang-wei;MA Qing-qing;SU Yong-heng;ZHANG Rong-jie(Henan Provincial Center for Disease Control and Prevention,Zhengzhou,Henan 450016,China)

机构地区：[1]河南省疾病预防控制中心,河南郑州450016

出　　处：《中国卫生检验杂志》2022年第3期284-287,共4页Chinese Journal of Health Laboratory Technology

基　　金：河南省重点研发与推广专项项目(192102310406)。

摘　　要：目的建立一种超高效液相色谱-三重四极杆串联质谱快速检测酵米面中米酵菌酸和毒黄素的确证方法。方法样品经乙腈提取后,采用Qu ECh ERS方法净化,取上清液氮吹至干,10%乙腈水复溶,过0.20μm尼龙滤膜上机检测。色谱分离采用ACQUITY HSS T3色谱柱,乙腈-2 mmol/L乙酸铵溶液体系梯度洗脱,质谱部分采用正负离子切换扫描-多反应监测(MRM)模式进行信息采集,对待测组分进行定性定量分析。结果米酵菌酸和毒黄素在0.5 ng/ml~50.0 ng/ml质量浓度内线性关系良好,相关系数分别为0.9992和0.9994。高、中、低3个浓度水平的平均加标回收率在88.7%~101.5%,相对标准偏差(RSD)为0.7%~2.8%,米酵菌酸和毒黄素的方法检出限分别为0.5μg/kg和0.25μg/kg。结论该方法具有样品前处理简单,灵敏高,准确性好及确证性强等特点,可以用于酵米面中米酵菌酸和毒黄素的同时测定。Objective An ultra-performance liquid chromatography-triple quadrupole tandem mass spectrometric method(UPLC-MS/MS)was established for the detection of bongkrekic acid and toxoflavin in ferment corn flour.Methods Bongkrekic acid and toxoflavin in samples were extracted by acetonitrile and cleaned up by Qu ECh ERS.After centrifugation,the supernatant was dried by nitrogen and redissolved by 10%acetonitrile-water solution.Target compounds,which were separated on a ACQUITY HSS T3 column using acetonitrile-2 mmol/L ammonium acetate solution as mobile phase,were identified in multiple reaction monitoring(MRM)mode and quantified by external standard method.Results The calibration curves for bongkrekic acid and toxoflavin both had a good linearity in the range of 0.5 ng/ml-50.0 ng/ml and the correlation coefficients(r)were 0.9992 and 0.9994.The average recoveries were in the range of 88.7%-101.5%,with relative standard deviations(RSD)of 0.7%-2.8%.The limits of detection for ricin and toxanthin were 0.5μg/kg and0.25μg/kg,respectively.Conclusion The method is rapid,sensitive,accurate and highly confirmatory,which can provide the final confirmation method for simultaneously detection of bongkrekic acid and toxoflavin in ferment corn flour.

关 键 词：酵米面 米酵菌酸 毒黄素 串联质谱 

分 类 号：O657.63[理学—分析化学]