4′,7-二乙基射干苷元合成产物中杂质的分离纯化及鉴定  

Isolation,Purification and Identification of the Impurities in the Synthesis Products of 4′,7-Diethyl Tectorigenin

作　　者：袁崇均[1] 陈雏[1] 陈帅[1] 罗森[1] 罗恒[1] 王笳[1] YUAN Chongjun;CHEN Chu;CHEN Shuai;LUO Sen;LUO Heng;WANG Jia(Institute of TCM Pharmacy,Sichuang Academy of Chinese Materia Medica,Chendu 610041,China)

机构地区：[1]四川省中医药科学院中药药学研究所,成都610041

出　　处：《中国药房》2018年第23期3208-3212,共5页China Pharmacy

基　　金：四川省科技计划项目(No.2016JY0009);四川省公益性科研院所基本科研业务项目(No.A-2017N-28)

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。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.

关 键 词：4′ 7-二乙基射干苷元 杂质 液相色谱-串联质谱法 鉴定 纯化 

分 类 号：R284.2[医药卫生—中药学] Q946.91[医药卫生—中医学]