【摘要】：α-二羰基化合物(α-DCs)如2,3-丁二酮(也稱雙乙酰)、2,3-戊二酮、乙二醛、甲基乙二醛、苯基乙二醛等,作為重要的風(fēng)味物質(zhì)存在于多種食品中；或作為代謝中間產(chǎn)物存在于人體生理系統(tǒng)中。研究表明,其在體內(nèi)大量積累與人類多種疾病的產(chǎn)生有關(guān),如糖尿病、腎病、阿爾茲海默癥等。關(guān)于α-DCs定性、定量檢測(cè)的研究有許多,盡管這些方法能夠滿足多方面分析需求,但仍有必要開(kāi)發(fā)新的方法來(lái)達(dá)到提高檢測(cè)速度及靈敏度等目的。本文以3,3'-二氨基聯(lián)苯胺(DAB)及其單丁二酮衍生物DAB-dia為衍生化試劑,建立了高靈敏度的柱前衍生.-HPLC方法快速測(cè)定酒類樣品中的2,3-丁二酮。通過(guò)實(shí)驗(yàn)確定了衍生化及HPLC測(cè)定條件。以DAB為衍生化試劑時(shí)：DAB鹽酸鹽大量過(guò)量(與2,3-丁二酮比例≥10：1),室溫下與2,3-丁二酮在水中反應(yīng)5min；以DAB-dia為衍生化試劑時(shí)：DAB-dia過(guò)量(與2,3-丁二酮比例大于10：1),室溫下與2,3-丁二酮在水中反應(yīng)10min即可。HPLC測(cè)定條件均為：ODS色譜柱,甲醇/水梯度洗脫(0～10min,6005～100%甲醇,10-15min,100%～60%甲醇,15-17min,60%甲醇),檢測(cè)波長(zhǎng)254nm。以DAB為衍生化試劑時(shí),2,3-丁二酮濃度在0.18μM-118.82μM范圍內(nèi)線性良好,R2=0.9992；檢測(cè)限0.09μM,定量限0.181μM；多次測(cè)定的RSD(%)值在0.06-1.35間,方法重現(xiàn)性及精密度均良好；以該方法測(cè)定了白酒二鍋頭和東北窖中2,3-丁二酮含量,分別為23.41μM和1.55μM,回收率為85.2%-103.6%。DAB-dia為衍生化試劑時(shí),2,3-丁二酮濃度在0.1μM-100μM范圍內(nèi)線性良好,R2=0.9991；檢測(cè)限與定量限分別為0.02μM和0.1μM,多次測(cè)定的RSD(%)值在1.3-3.7間,方法重現(xiàn)性及精密度均良好；成功檢測(cè)了5種啤酒中2,3-丁二酮含量,回收率為81.7%-88.5%,說(shuō)明方法準(zhǔn)確度高。綜上所述,DAB與DAB-dia作為衍生化試劑測(cè)定2,3-丁二酮具有反應(yīng)條件簡(jiǎn)單、反應(yīng)速度快、測(cè)定靈敏度高、準(zhǔn)確度好的優(yōu)勢(shì),因此可進(jìn)一步發(fā)展成為檢測(cè)食品、飲料及生物樣品中2,3-丁二酮及α-DCs的高效方法。
[Abstract]:偽 -dicarbonyl compounds (偽-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 偽-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，

本文編號(hào)：2312133