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作 者:吴新文 吴华秀 于以竹 黄永桥 张世芹 田乙卜 曹俊杰 杨昌彪 WU Xinwen;WU Huaxiu;YU Yizhu;HUANG Yongqiao;ZHANG Shiqin;TIAN Yibo;CAO Junjie;YANG Changbiao(Guizhou Testing Technology Research and Application Center,Guiyang 550002,China;Guizhou Academy of Testing and Analysis,Guiyang 550002,China)
机构地区:[1]贵州省检测技术研究应用中心,贵州贵阳550002 [2]贵州省分析测试研究院,贵州贵阳550002
出 处:《贵州科学》2022年第5期5-11,共7页Guizhou Science
基 金:黔科院J字〔2021〕38号。
摘 要:利用两泵一阀加两种检测器的液相色谱分析系统,建立在线SPE-HPLC-紫外串联荧光检测器同时测定抹茶中的叶黄素、β-胡萝卜素和维生素E的方法。样品经皂化后,以高聚合物为填料的具有耐强碱溶液能力的PLRP-S色谱柱作为固相萃取柱,对样品皂化液进行在线净化,以PFP色谱柱梯度洗脱分离目标物,将紫外和荧光检测器串联,同时测叶黄素、β-胡萝卜素和维生素E。采用保留时间定性,外标法定量。利用样品和标准品对建立的方法进行方法学验证,各目标物在各自浓度范围内线性良好,在三个水平进行加标回收试验,回收率在87.0%~112%之间,相对标准偏差(RSD)在1.5%~5.6%之间,方法检出限为0.004~0.020 mg/kg之间。该方法具有操作简单、准确、灵敏度高等优点,适合批量样品的快速测定。Using a liquid chromatographic analysis system with two pumps,one valve and two detectors,a method for the simultaneous determination of lutein,β-carotene and vitamin E in matcha by the online SPE-HPLC-ultraviolet tandem fluorescence detector is established.After the sample is saponified,the PLRP-S column with strong alkali resistance and high polymer as the filler is used as the solid-phase extraction column,the sample saponification solution is purified online,the target substances are separated by PFP column gradient elution,and the ultraviolet and fluorescent detectors are connected in series to measure the contents of lutein,β-carotene and vitamin E at the same time.The retention time is used for qualitative analysis and the external standard method is used for quantitative analysis.The established method is methodologically verified by samples and standard substances.The results show that each target substance is linear in its own concentration range,and the spiked recovery rates at three levels are between 87.0%and 112%,the relative standard deviations(RSD)are between 1.5%and 5.6%,and the limits of detection of the method are between 0.004 mg/kg and 0.020 mg/kg.The method has the advantages of simple operation,high accuracy and high sensitivity,and is suitable for the rapid determination of batch samples.
关 键 词:在线SPE-HPLC-紫外串联荧光检测器 抹茶 叶黄素 Β-胡萝卜素 维生素E
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