柱前衍生-HPLC法测定2,3-丁二酮的研究
发布时间：2018-11-05 12:47
【摘要】：α-二羰基化合物(α-DCs)如2,3-丁二酮(也称双乙酰)、2,3-戊二酮、乙二醛、甲基乙二醛、苯基乙二醛等,作为重要的风味物质存在于多种食品中；或作为代谢中间产物存在于人体生理系统中。研究表明,其在体内大量积累与人类多种疾病的产生有关,如糖尿病、肾病、阿尔兹海默症等。关于α-DCs定性、定量检测的研究有许多,尽管这些方法能够满足多方面分析需求,但仍有必要开发新的方法来达到提高检测速度及灵敏度等目的。本文以3,3'-二氨基联苯胺(DAB)及其单丁二酮衍生物DAB-dia为衍生化试剂,建立了高灵敏度的柱前衍生.-HPLC方法快速测定酒类样品中的2,3-丁二酮。通过实验确定了衍生化及HPLC测定条件。以DAB为衍生化试剂时：DAB盐酸盐大量过量(与2,3-丁二酮比例≥10：1),室温下与2,3-丁二酮在水中反应5min；以DAB-dia为衍生化试剂时：DAB-dia过量(与2,3-丁二酮比例大于10：1),室温下与2,3-丁二酮在水中反应10min即可。HPLC测定条件均为：ODS色谱柱,甲醇/水梯度洗脱(0～10min,6005～100%甲醇,10-15min,100%～60%甲醇,15-17min,60%甲醇),检测波长254nm。以DAB为衍生化试剂时,2,3-丁二酮浓度在0.18μM-118.82μM范围内线性良好,R2=0.9992；检测限0.09μM,定量限0.181μM；多次测定的RSD(%)值在0.06-1.35间,方法重现性及精密度均良好；以该方法测定了白酒二锅头和东北窖中2,3-丁二酮含量,分别为23.41μM和1.55μM,回收率为85.2%-103.6%。DAB-dia为衍生化试剂时,2,3-丁二酮浓度在0.1μM-100μM范围内线性良好,R2=0.9991；检测限与定量限分别为0.02μM和0.1μM,多次测定的RSD(%)值在1.3-3.7间,方法重现性及精密度均良好；成功检测了5种啤酒中2,3-丁二酮含量,回收率为81.7%-88.5%,说明方法准确度高。综上所述,DAB与DAB-dia作为衍生化试剂测定2,3-丁二酮具有反应条件简单、反应速度快、测定灵敏度高、准确度好的优势,因此可进一步发展成为检测食品、饮料及生物样品中2,3-丁二酮及α-DCs的高效方法。
[Abstract]:伪 -dicarbonyl compounds (伪-DCs), such as 2o 3-butanedione (diacetyl), 2o 3-pentanedione, Glyoxal, methyl Glyoxal, phenyl Glyoxal, exist as important flavor substances in many kinds of foods. Or as a metabolic intermediate in the human physiological system. Studies have shown that its accumulation in the body is associated with the production of many diseases, such as diabetes, nephropathy, Alzheimer's disease and so on. There are many studies on the qualitative and quantitative detection of 伪-DCs. Although these methods can meet the needs of many aspects of analysis, it is still necessary to develop new methods to improve the detection speed and sensitivity. In this paper, a high sensitivity precolumn derivatization method was established using (DAB) and its derivative of monobutylene dianiline (DAB-dia) as derivatization reagents.-HPLC method for the rapid determination of 2h3- butanedione in wine samples was developed. The conditions of derivatization and HPLC determination were determined by experiments. When DAB was used as derivatization reagent, a large amount of DAB hydrochloride (the ratio of 2o 3-butanedione 鈮，
本文编号：2312133
[Abstract]:伪 -dicarbonyl compounds (伪-DCs), such as 2o 3-butanedione (diacetyl), 2o 3-pentanedione, Glyoxal, methyl Glyoxal, phenyl Glyoxal, exist as important flavor substances in many kinds of foods. Or as a metabolic intermediate in the human physiological system. Studies have shown that its accumulation in the body is associated with the production of many diseases, such as diabetes, nephropathy, Alzheimer's disease and so on. There are many studies on the qualitative and quantitative detection of 伪-DCs. Although these methods can meet the needs of many aspects of analysis, it is still necessary to develop new methods to improve the detection speed and sensitivity. In this paper, a high sensitivity precolumn derivatization method was established using (DAB) and its derivative of monobutylene dianiline (DAB-dia) as derivatization reagents.-HPLC method for the rapid determination of 2h3- butanedione in wine samples was developed. The conditions of derivatization and HPLC determination were determined by experiments. When DAB was used as derivatization reagent, a large amount of DAB hydrochloride (the ratio of 2o 3-butanedione 鈮，
本文编号：2312133
本文链接：https://www.wllwen.com/kejilunwen/huaxue/2312133.html
教材专著
