基于UPLC-DAD-CAD双检测器串联的DON纯度测量方法对比研究  

Comparative Study on DON Purity Analysis Based on UPLC with DAD Coupled to CAD

作　　者：王松山 雷达 贾睿晖 李丽 周明慧 王松雪 WANG Songshan;LEI Da;JIA Ruihui;LI Li;ZHOU Minghui;WANG Songxue(Academy of National Food and Strategic Reserves Administration,Beijing 100037,China;KangYuan TechBio Co.,Ltd,Beijing 102600,China;Beijing City University,Beijing 100083,China)

机构地区：[1]国家粮食和物资储备局科学研究院,北京100037 [2]北京康源泰博生物科技有限公司,北京102600 [3]北京城市学院,北京100083

出　　处：《计量学报》2024年第7期1081-1088,共8页Acta Metrologica Sinica

基　　金：国家重点研发计划(2022YFF0710400)。

摘　　要：通过串联二极管阵列检测器(DAD)和电雾式检测器(CAD),建立了脱氧雪腐镰刀菌烯醇(DON)纯度分析的液相色谱方法,优化的色谱条件为6%甲醇等度洗脱20 min。2种检测器测得的杂质种类和含量存在明显不同,其中DAD识别到杂质17个,以杂质15含量最高(0.847%),杂质17次之(0.0812%),其次为杂质2、5和8(大于0.01%);CAD识别到杂质9个,以杂质17含量最高(0.4060%),杂质15次之(0.3499%),其次为杂质10、11和12(大于0.1%)。DAD方法测得纯度为98.92%,显著高于CAD方法的结果(98.61,p<0.001);且相对标准偏差(0.00670%)也较CAD方法低(0.0461%)。DAD方法的纯度不确定度为0.463%,主要由杂质响应差异引入;CAD方法为0.0503%,主要由测量重复性引入。研究结果或可为DON纯度分析提供技术支撑。An ultra-high performance liquid chromatography with diode array detector coupled to charged aerosol detector(UPLC-DAD/CAD)method was established for comparative study on deoxynivalenol(DON)purity analysis.The optimized chromatographic condition was isocratic elution with 6%methanol for 20 minutes.There were obvious differences in the types and amounts of impurities detected by the two detectors.17 impurities were identified by DAD with impurity 15 accounting for the highest proportion(0.847%),following by impurity 17(0.0812%)and impurities 2,5 and 8(above 0.01%).9 impurities were identified by CAD with impurity 17 accounting for the highest proportion(0.4060%),following by impurity 15(0.3499%)and impurities 10,11 and 12(above 0.1%).The purity obtained by DAD detection method was 98.92%,significantly higher than that obtained by CAD detection method(98.61,p<0.001).And the relative standard deviation of DAD method(0.00670%)was also lower than that of the CAD method(0.0461%).The measurement uncertainty of purity by the DAD method was 0.463%,mainly introduced by response differences of the impurities;while it was 0.0503%for the CAD method,which was mainly introduced by measurement repeatability.The results may be helpful for the chromatographic purity analysis of DON.

关 键 词：生物计量 脱氧雪腐镰刀菌烯醇 C DAD CAD 不确定度 

分 类 号：TB99[一般工业技术—计量学]