4′ ,7-二乙基射干苷元合成产物中杂质的分离纯化及鉴定
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篇名: 4′ ,7-二乙基射干苷元合成产物中杂质的分离纯化及鉴定
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摘要: 目的:分离纯化并鉴定4′ ,7-二乙基射干苷元合成产物中的杂质,为其质量控制提供依据。方法:采用液相色谱-串联质谱法分析4′ ,7-二乙基射干苷元合成产物中的杂质,然后根据各杂质离子峰的质荷比[M+H]+推定其可能结构;采用硅胶柱层析,以氯仿-甲醇(梯度洗脱,20 ∶ 1、10 ∶ 1、8 ∶ 1、6 ∶ 1、5 ∶ 1、3 ∶ 1、2 ∶ 1、1 ∶ 1、0 ∶ 1,V/V)分离纯化部分杂质,并采用紫外、红外、核磁共振波谱等技术鉴定其结构。结果:在4′ ,7-二乙基射干苷元合成产物中共检出21个杂质,推定出17个杂质的可能结构;分离纯化得到4个杂质单体,分别鉴定为2-羟基-3-甲氧基-4,6,4′ -三乙氧基脱氧安息香(1)、2,6-二羟基-3-甲氧基-4,4′ -二乙氧基脱氧安息香(2)、射干苷元(3)和射干苷(4),其中杂质2为新化合物。结论:本结果可为4′ ,7-二乙基射干苷元的合成工艺优化及质量控制提供重要依据。
ABSTRACT: OBJECTIVE: To isolate, purify and identify the impurities in the synthesis products of 4′ ,7-diethyl tectorigenin, and to provide reference for its quality control. METHODS: LC-MS/MS was adopted to analyze the impurities in the synthesis products of 4′ ,7-diethyl tectorigenin; the potential structure of each impurity was deduced according to mass-charge ratio [M+H]+ of ion peak. The major impurities were isolated by silica gel column chromatography using chloroform-methanol (gradient elution, 20 ∶ 1, 10 ∶ 1, 8 ∶ 1, 6 ∶ 1, 5 ∶ 1, 3 ∶ 1, 2 ∶ 1, 1 ∶ 1, 0 ∶ 1, V/V). The structures of the impurities were identified by UV spectroscopy, IR spectroscopy and NMR. RESULTS: Totally 21 impurities were detected in the synthesis products of 4′ ,7-diethyl tectorigenin. The potential structures of 17 impurities were elucidated; 4 impurity monomers were isolated and purified. The impurities were identified as 2-hydroxy-3-methoxy-4,6,4′ -triethoxy deoxybenzoin (1), 2,6-dihydroxy-3-methoxy-4,4′ -diethoxy deoxybenzoin (2), tectorigenin (3) and tectoridin (4). impurity 2 was reported for the first time. CONCLUSIONS: The result can provide important evidence for the optimization of synthesis process and quality control of 4′ ,7-diethyl tectorigenin.
期刊: 2018年第29卷第23期
作者: 袁崇均,陈雏,陈帅,罗森,罗恒,王笳
AUTHORS: YUAN Chongjun,CHEN Chu,CHEN Shuai,LUO Sen,LUO Heng,WANG Jia
关键字: 4′ ,7-二乙基射干苷元;杂质;液相色谱-串联质谱法;鉴定;纯化
KEYWORDS: 4′ ,7-diethyl tectorigenin; Impurity; LC-MS/MS; Identification; Putification
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