反溶剂重结晶法制备萘普生超细微粒  

Preparation of Ultra-Fine Naproxen Particles by Anti-Solvent Recrystallization

作　　者：宋湘玲[1] 王洁欣[1] 陈建峰[1] 沈志刚[1,2] Jimmy Yun 

机构地区：[1]中新国际纳米技术工程研究中心纳米材料先进制备技术与应用科学教育部重点实验室,北京化工大学,北京100029 [2]新加坡纳米材料科技有限公司,新加坡139944

出　　处：《化学反应工程与工艺》2007年第3期212-216,共5页Chemical Reaction Engineering and Technology

基　　金：国家自然科学杰出青年基金(20325621)

摘　　要：在溶剂(丙酮)-反溶剂(水)体系下,采用反溶剂重结晶法制备了超细萘普生微粒。研究了不同溶剂-反溶剂体积比、重结晶温度、表面活性剂用量及陈化条件对重结晶产物粒径和形貌的影响。采用扫描电子显微镜(SEM)、表面吸附(BET)、红外光谱(IR)、X射线衍射(XRD)等检测手段对原料药和重结晶产物进行了对比分析。实验结果表明,当溶剂与反溶剂体积比为1:20,重结晶温度为4～8℃,表面活性剂聚乙烯吡咯烷酮(PVP)的质量分数为0.5%～1.0%,60℃下陈化2 h时。可得到短径300～500 nm,长径1～2μm的超细萘普生粉体。重结晶所得产物的晶型和物理性质均未发生变化,但粒度显著减小,形貌趋于规整且比表面积增加至原料药的5.3倍。Ultra-fine naproxen particles were preparated by anti-solvent recrystallization. The main factors which influenced the mean particle size and morphology, such as ratio of solvent to anti-solvent, recrystallization temperature, aging condition and surfactant content, were investigated experimentally. Scan Electronic Microscope （SEM）, Brunauer-Emmett-Teller （BET）, Infrared （IR） and X-Ray Diffraction （XRD） were employed to characterize the as-prepared product and raw drug. The results showed that ultra-fine naproxen particles with a rod-like shape with a width of 300--500 nm and a length of 1-2 gm could be prepared under the conditions of the solvent to antisolvent ratio of 1 ： 20, recrystallization of 4--8℃, surfactants （PVP） mass content of 0.5%--1.0% and aging at 60 ℃ for 2 h. In addition, the crystallization process would not change the drug＇s physicochemical properties and crystal form. Due to the smaller particle size, the BET special surface of ultra-fine naproxen was about 5.3 times as much as that of the commercial crude drug.

关 键 词：萘普生 溶剂 反溶剂 重结晶 超细粉体 

分 类 号：TQ456.1[化学工程—农药化工]