脂质立方液晶辅料植烷三醇的合成研究  

Synthesis of Phytanetriol as a Lipid Cubic Liquid Crystal Excipient

作　　者：饶信权 张锐 RAO Xinquan;ZHANG Rui(Key Laboratory of Modern Preparation of Chinese Medicine,Jiangxi University of Chinese Medicine,Nanchang 330004,China)

机构地区：[1]江西中医药大学,现代中药制剂教育部重点实验室,南昌330004

出　　处：《中国药学杂志》2024年第12期1093-1099,共7页Chinese Pharmaceutical Journal

基　　金：国家自然科学基金项目资助(82360702,81560579,81160523);江西省教育厅科技项目资助(GJJ14609);江西中医药大学校级科技创新团队发展项目资助(CXTD22005,20045252300403)。

摘　　要：目的建立以植醇为原料,低浓度的过氧化氢为氧化剂,甲酸为载氧剂,在无催化剂的条件下,通过环氧化/开环反应合成植烷三醇的方法。方法采用单因素试验,考察甲酸、过氧化氢与植醇的摩尔比、反应温度和时间对植烷三醇收率的影响,并进行3批次重复性验证。用气-质联用仪、红外光谱仪以及核磁共振波谱仪对植烷三醇的色谱纯度和结构进行了分析。结果最佳工艺条件确定为:环氧化反应体系最佳条件为n(HCOOH)-n(H_(2)O_(2))n-n(植醇)=5∶1.3∶1,温度55℃,时间2 h;开环反应体系最佳条件为pH值13,温度105℃,时间0.5 h。经验证实验,该法植烷三醇合成工艺产率可达86.6%,色谱纯度为94.6%。结论所建立的合成方法工艺稳定,质量可控,并且所合成的植烷三醇纯度优于市售产品。OBJECTIVE To synthesize phytanetriol by epoxidation/ring-opening reaction under catalyst-free conditions using phytol as raw material,low concentration of hydrogen peroxide as oxidant,and formic acid as oxygen carrier.METHODS The effects of the molar ratios of formic acid and hydrogen peroxide to phytol,reaction temperature,and reaction time on the yield of phytanetriol were investigated using a single-factor test and verified by 3-batch reproducibility.The chromatographic purity and structure of phytanetriol were analyzed by gas-mass spectrometry,infrared spectroscopy,and nuclear magnetic resonance spectrometry.RESULTS The optimal conditions for the epoxidation reaction system were n(HCOOH):n(H_(2)O_(2)):n(phytol)=5∶1.3∶1,temperature 55℃,and reaction time 2 h.The optimal conditions for the ring-opening reaction system were pH=13,temperature 105℃,and reaction time 0.5 h.The phytanetriol synthesis process had a yield of 86.6%in the validated experiments.The chromatographic purity was 94.6%.CONCLUSION The synthesis process is stable and can produce phytanetriol with controllable quality and better purity than commercially available products.

关 键 词：脂质立方液晶 植烷三醇 过氧化氢 环氧化反应 开环反应 

分 类 号：R914[医药卫生—药物化学]