Preparation and evaluation of monolithic molecularly imprinted stationary phase for S-naproxen

An S-naproxen (S-NAP) molecularly imprinted monolithic stationary phase (MIMSP) with specific recognition for S-NAP and naproxen (NAP) was prepared by in situ technique,utilizing 4-vinylpridine (4-VP) ...     

两亲性聚乙二醇接枝聚乳酸胶束的制备及特性

制备聚乙二醇接枝聚乳酸(PPLA)聚合物胶束,探讨其作为药物载体的可行性和稳定性。溶剂挥发法制备PPLA胶束并对其表征。萘普生为模型药物,单因素考察了投药量、丙酮用量、加样顺序对包封率的影响。结果表明,PPLA临界胶束质量浓度(CMC)低,为3×10-4g/L;胶束呈球形、平均粒径小于200nm;在室温、稀释、碱性条件下稳定;最佳载药条件为:材料与药物同时溶于丙酮后滴入水中、丙酮与水的体积比1∶10,萘普生与PPLA质量比0.8∶10,PPLA胶束质量浓度1.0g/L。37℃时载药胶束在磷酸盐缓冲液(PBS)中可缓慢持续释放5d以上。结果证明,制备的聚乙二醇接枝改性聚乳酸聚合物胶束可用作疏水性药物的缓释给药载体。     

Chromatographic Separation of Naproxen Enantiomers using Hydroxypropyl‐β‐Cyclodextrin as Chiral Mobile Phase Additive

Abstract

Chromatographic separation of naproxen has been studied using hydroxypropyl‐β‐cyclodextrin as chiral mobile phase additive. The effects of mobile‐phase composition were researched in detail. The appropriate composition of mobile phase was 85:15 (v/v) aqueous with 0.5% TEA at pH 3.5/ ethanol containing 25 mM HP‐β‐CD, and the column temperature was set of 25°C. Graphs of 1/k versus [HP‐β‐CD] gave good linear relationships, indicating the stoichiometry ratio of naproxen with HP‐β‐CD of 1:1. Apparent thermodynamic parameters were also calculated from the plots of lnα versus 1/T, it was found that the enantioseparation was enthalpy driven and the inclusion process was exothermic.     

萘普生稀土配合物的合成与表征

制备了萘普生与稀土元素镨、镝、铒的配合物。通过元素分析、摩尔电导、红外光谱及热分析等方法进行了表征。结果表明,配合物的组成为:RE·L3·H2O(RE=Pr、Er、Dy),其中心离子的配位数为7。     

MCM-41表面接枝过渡金属（Co^2＋，Ni^2＋）对萘普生吸附性能的影响

在氨基化MCM-41表面引Co^2＋,Ni^2＋,作为吸附剂来去除水中的萘普生．氨基化MCM-41用X射线衍射、氮气吸／脱附曲线、红外光谱和热重分析表征．吸附萘普生的实验在室温25℃下进行．材料的吸收能力顺序为：NiNH2-MCM-41〉CoNH2-MCM-41．该吸附结果与材料的结构和性质有关,材料的氨基化高度依赖于嫁接过程的性质和金属的选择．     

萘普生分子印迹拆分过程热力学研究

采用4-乙烯基吡啶为功能单体,三甲氧基丙烷三甲基丙烯酸酯为交联剂,制备出(S)-萘普生的分子印迹聚合物,并将其用作高效液相色谱固定相,对其进行了评价.研究了流动相流速、不同功能单体和柱温对拆分效果的影响,测定出分离过程的热力学参数,证明萘普生分子印迹拆分过程是焓控过程.     

高效液相色谱-二极管阵列法测定保健酒中的萘普生

近期不断发现抗炎药物被违法添加到抗风湿保健酒中增加治疗效果,这种现象对消费者健康构成威胁。萘普生是常用非甾体抗炎药物,本研究建立保健食品中违禁添加萘普生的液相检测方法。通过酸性条件氯仿和碱性水溶液两步液-液萃取,从保健酒中提取和净化萘普生。使用Kromasil 100-5C18(250×4.6 mm E74572)色谱柱,以甲醇-0.01M磷酸缓冲液(pH 3.0)(75/25,V/V)流动相,流速为1.0 mL/min进行分离;检测波长为231 nm。通过比对色谱峰保留值和加标实验,结合二极管阵列扫描图谱对可疑样品定性,并根据外标法峰面积定量检测萘普生含量。检品和基质成分基本实现了基线分离,最低检测限为0.5μg/mL,工作曲线的线性范围:5~80μg/mL(R2=0.9993),RSD为1.87%(n=6),加标回收率83.3~92.6%。方法准确、可靠,适用于检测保健品中违法添加的萘普生。     

d-萘普生中间体2-(6’-甲氧基-2’-萘基)丙烯酸合成方法的研究

以丙酮酸乙酯 (Ⅱ )和 2 萘甲醚 (Ⅰ )为原料 ,在AlCl3 催化下反应合成了 2 羟基 2 (6’ 甲氧基 2’ 萘基 )丙酸乙酯 (Ⅲ )。最佳反应条件为 :n(Ⅱ )∶n(Ⅰ ) =1 2∶1 ,反应温度为 0～ 5℃ ,反应时间为 1 5h。Ⅲ经碱催化水解 32h得 2 羟基 2 (6’ 甲氧基 2’ 萘基 )丙酸 (Ⅳ ) ,此两步反应收率为 74 8%。Ⅳ经酸催化脱水得 2 (6’ 甲氧基 2’ 萘基 )丙烯酸 (Ⅴ ) ,收率为 84.6 %。Ⅴ经立体加氢即得d 萘普生 (Ⅵ )。     

Conductive‐diamond electrochemical advanced oxidation of naproxen in aqueous solution: optimizing the process

BACKGROUND: Electrochemical advanced oxidation treatment using boron‐doped diamond (BDD) electrodes is a promising technology to treat small amounts of toxic and biorefractory pollutants in water. This process has been tested on the degradation of naproxen, a common pollutant drug present in surface waters. To optimize the process a series of experiments have been designed to study the interaction between four variables: pH (over the range 5–11); current (0–320 mA cm^?2); supporting Na₂SO₄ electrolyte concentration (0–0.375 mol L^?1); and solution flow rate (Q_v) between 3.64 and 10.8 cm³ min^?1. RESULTS: Among these variables the influence of current was the greatest, the second was the salt concentration, the third flow rate, and the fourth pH. An ANOVA test reported significance for seven of the fourteen variables involved and the degradation of naproxen was optimized using response surface methodology. CONCLUSIONS: Optimum conditions for naproxen removal (100%) were found to be pH = 10.70, Q_v = 4.10 cm³ min^?1, current density = 194 mA cm^?2 using a supporting electrolyte concentration of 0.392 mol L^?1. Copyright © 2010 Society of Chemical Industry     

多级离心逆流萃取萘普生对映体模拟及实验研究

基于萘普生(NAP)对映体的单级手性萃取数学模型和质量守恒定律,建立了多级离心逆流萃取萘普生对映体数学模型。采用Matlab语言编写程序模拟了相比、萃取剂浓度、水相pH值等参数对萃取相出口对映体过剩量和产率的影响,并经实验研究对模型模拟进行验证。结果表明:采用中间进料,对映体浓度[R,S-NAP]=0.025 mol·L^-1、萃取剂浓度[C]=0.050 mol·L^-1、相比W/O=7、水相pH=2.5、温度T=5℃时,经10级离心逆流萃取后萃取相出口S-NAP对映体过剩量为45%,相应的产率60%,实验结果和模型模拟值符合得很好。