本文選題：4-氯扁桃酸 + 萃取拆分��； 參考：《華東理工大學》2017年碩士論文

【摘要】：論文以外消旋4-氯扁桃酸(4-ClMA)為研究對象,研究了兩種不同體系中4-ClMA對映體的手性選擇性萃取拆分特性,研究內(nèi)容如下:論文首先建立了以羥丙基-β-環(huán)糊精(HP-β-CD)為手性添加劑,以C18柱為固定相,反相液相色譜體系下手性流動相添加劑法拆分分析4-氯扁桃酸對映體的方法,通過考察流動相組成、手性添加劑的濃度、緩沖鹽的含量等影響因素,優(yōu)化得到了相應的HPLC分析條件,在此條件下,4-ClMA對映體的分離度大于1.5,實現(xiàn)了基線分離。論文從精密度、線性、檢測限和定量限等幾個方面,對所建立的4-ClMA對映體的定量分析方法進行了驗證。其次研究了水相/有機相體系中4-ClMA對映體的萃取拆分特性,選擇的手性拆分劑分別為酒石酸衍生物和氨基酸衍生物。其中酒石酸衍生物中以D-(+)-二對甲苯甲酰氧基丁二酸(D-DTTA)為手性拆分劑的萃取拆分效果最佳,分離因子可達1.22。氨基酸衍生物中以2-氯苯甲氧基羰基纈氨酸(2-Cl-Z-纈氨酸)為手性拆分劑的萃取拆分效果最佳,分離度因子達到3.05。論文分別對對兩種手性拆分劑的萃取拆分的有關(guān)影響因素如有機溶劑種類、水相pH值、拆分劑種類及濃度、4-ClMA濃度和萃取溫度進行了考察,分析了相應的萃取拆分機理。最后研究了聚乙二醇/硫酸銨雙水相體系中4-ClMA對映體的萃取拆分特性,所使用的手性拆分劑為HP-β-CD。論文分析了雙水相體系拆分4-氯扁桃酸對映體的機理,考察了 pH、聚乙二醇分子量、聚乙二醇的質(zhì)量分數(shù)、硫酸銨質(zhì)量分數(shù)、羥丙基-β-環(huán)糊精、4-氯扁桃酸濃度以及萃取溫度對拆分效果的影響,在優(yōu)化的萃取拆分條件下,4-ClMA對映體的分離因子達到1.61。
[Abstract]:The chiral selective extraction and resolution of 4-ClMA enantiomers in two different systems were studied. The results are as follows: firstly, hydroxypropyl 尾 -cyclodextrin (HP- 尾 -CDCD) was used as chiral additive. Using C18 column as stationary phase, the chiral mobile phase additive was used to separate and analyze the enantiomers of 4-chloromandelic acid in reversed phase liquid chromatographic system. The influence factors such as the composition of mobile phase, the concentration of chiral additive and the content of buffer salt were investigated. The corresponding HPLC analysis conditions were obtained, under which the separation degree of 4-ClMA enantiomers was greater than 1.5, and the baseline separation was realized. In this paper, the quantitative analysis method of 4-ClMA enantiomers is verified from the aspects of precision, linearity, detection limit and quantitative limit. Secondly, the extraction and resolution properties of 4-ClMA enantiomers in aqueous / organic phase system were studied. The chiral resolution agents were tartaric acid derivatives and amino acid derivatives, respectively. Among the tartaric acid derivatives, D-dimethylformyl succinic acid D-DTTAwas the best extraction and resolution agent, and the separation factor was 1.22. In amino acid derivatives, 2-chlorobenzene methoxycarbonyl valine (2-Cl-Zvaline) is the best chiral separation agent, and the separation factor is 3.05. In this paper, the factors affecting the extraction and resolution of two chiral resolution agents, such as the kinds of organic solvents, the pH value of aqueous phase, the kinds and concentrations of the resolution agents, the concentration of 4-ClMA and the extraction temperature, were investigated, and the corresponding mechanism of extraction and resolution was analyzed. Finally, the extraction and resolution properties of 4-ClMA enantiomers in polyethylene glycol / ammonium sulfate aqueous two-phase system were studied. The chiral resolution agent was HP- 尾 -CD. The mechanism of enantiomeric separation of 4-chloromandelic acid by aqueous two-phase system was analyzed. The pH, molecular weight of polyethylene glycol, mass fraction of polyethylene glycol, and mass fraction of ammonium sulfate were investigated. The effects of concentration of hydroxypropyl- 尾 -cyclodextrin 4-chloromandelic acid and extraction temperature on the resolution efficiency were investigated. The separation factor of 4-ClMA enantiomers was 1.61under the optimized conditions.
【學位授予單位】：華東理工大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O658.2;TQ460.1

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本文編號：1913793