左旋醋酸棉酚的制备、结构确证及定量分析  

Preparation,Structure Confirmation,and Quantitative Analysis of L-Gossypol Acetate

作　　者：张辉 刘滋烁 王宇 沈静 姚军[1,2] ZHANG Hui;LIU Zishuo;WANG Yu;SHEN Jing;YAO Jun(College of Pharmacy,Xinjiang Medical University,Urumqi 830011,China;Xinjiang Key Laboratory of Natural Medicines Active Components and Drug Release Technology,Urumqi 830011,China;Department of Pharmacy,The First Affiliated Hospital of Xinjiang Medical University,Urumqi 830054,China)

机构地区：[1]新疆医科大学药学院,新疆乌鲁木齐830011 [2]新疆天然药物活性组分与释药技术重点实验室,新疆乌鲁木齐830011 [3]新疆医科大学第一附属医院药学部,新疆乌鲁木齐830054

出　　处：《化学与生物工程》2025年第4期58-63,共6页Chemistry & Bioengineering

基　　金：国家自然科学基金项目(82360722);中央引导地方科技发展专项(ZYYD2023B11);新疆维吾尔自治区重大科技专项(2022A03007)。

摘　　要：利用手性拆分试剂拆分混旋醋酸棉酚,采用硅胶柱色谱分离后,经酸水解反应得到左旋醋酸棉酚粗品,并采用中压制备色谱进一步纯化;通过比旋度、紫外可见吸收光谱、红外光谱、高分辨质谱确证其结构;采用高效液相色谱、核磁共振氢谱测定其含量。结果表明,混旋醋酸棉酚经衍生化反应、硅胶柱色谱分离、酸水解反应、中压制备色谱纯化后得到左旋醋酸棉酚,结构准确,高效液相色谱法测得其含量为98.60%,核磁共振氢谱法测得其含量为97.64%。该分离制备纯化方法可成功得到较高纯度的左旋醋酸棉酚,结构确证和含量测定方法操作简便,准确高效。We prepared crude L-gossypol acetate through resolution of mixed gossypol acetate by chiral resolution reagent,separation by silica gel column chromatography,and acid hydrolysis reaction.Then,we further purified the L-gossypol acetate by medium-pressure preparative chromatography.Moerover,we confirmed the structure of L-gossypol acetate by specific rotation,UV-Vis absorption spectrum,IR spectrum,and HRMS spectrum.Furthermore,we determined the content of L-gossypol acetate by HPLC and 1 HNMR.The results show that L-gossypol acetate is prepared and purified by derivatization,silica gel column chromatography,acid hydrolysis,and medium-pressure preparative chromatography.The structure of L-gossypol acetate is accurate with content of 98.60%by HPLC and 97.64%by 1 HNMR,respectively.The high purity L-gossyrol acetate is successfully obtained by this separation,preparation,and purification method,and the structure confirmation and content determination methods are simple,accurate,and efficient.

关 键 词：左旋醋酸棉酚 结构确证 核磁共振氢谱 含量测定 

分 类 号：R917[医药卫生—药物分析学]