马来海松酸铜的合成及表征

本文以马来海松酸酐和醋酸铜为原料,合成了马来海松酸铜.研究了马来海松酸与醋酸锌的摩尔比、反应时间、反应温度对反应过程的影响.通过傅立叶红外光谱(FT-IR)、扫描电镜(SEM)、能谱仪(EDAX)和X-射线衍射(XRD)等对产物进行了分析和表征.结果表明:当马来海松酸和醋酸铜摩尔比为1∶4、反应温度为55℃、反应时间为5h时,产率可达97％以上.马来海松酸铜属于三维网状化合物,产物中的-COO-与Cu2发生了化学键合.同时拓宽了松香的应用范围,提高了松香的附加值.     

溴化马来松香的合成、表征及其阻燃性的研究

本文以马来松香与液溴加成,合成了溴化马来松香;研究了反应温度、原料的摩尔比、反应时间等因素对反应过程及产物性能的影响.用FT-IR、1H NMR和TG对溴化马来松香进行了表征.结果表明,当反应温度为-2～6℃,反应时间5～6 h,反应物的当量配比约为1.2时,收率可达87.9%.溴化马来松香具有较好的阻燃性,同时也拓宽了松香的应用范围,提高了松香的附加值.     

槐豆胶的流变性及与黄原胶的协效性研究

本文主要对槐豆胶的流变性及槐豆胶与黄原胶的协效增稠性和协效凝胶性进行了研究。结果表明:槐豆胶具有较高的粘度,当胶浓度为1％时,其粘度为660mpa·s;浓度、剪切力、温度、酸碱、冻融等变化与槐豆胶的粘度都有较大的关系;槐豆胶还有一非常显著的特性即是与黄原胶的协效增稠性和协效凝胶性,可作为理想的黄原胶的增稠剂和凝胶剂。     

石油树脂施胶剂的研制

以改性的石油树脂为原料,采用常压转相乳化法制备了石油树脂施胶剂。研究了物料用量、乳化剂、阻聚剂、温度、搅拌速度等因素对产品性能的影响,确定了最佳反应工艺条件:马来酸酐和石蜡用量分别为改性树脂质量的8%和6%,阳/非离子表面活性荆质量比1.5:1.0,用量为改性树脂质量的8%,阻聚剂用量为石油树脂质量的0.08%;马来酸酐与石油树脂的加成温度为180℃左右,乳化温度为150～160℃,转相温度为90～100℃,同时对所得产品进行了表征。     

普鲁兰酶改性瓜尔胶及其与黄原胶复配性能研究

通过红外光谱表征、稳态流动和动态应力扫描法考察了普鲁兰酶对瓜尔胶的脱支效应和改性瓜尔胶与黄原胶的复配性能。结果表明,普鲁兰酶不仅降低了瓜尔胶中半乳糖的含量,也降低了瓜尔胶的分子量及粘度,但未改变瓜尔胶主链的主体结构和糖苷键的构型,也未改变其流变学性质。与天然瓜尔胶-黄原胶复配胶相比,改性瓜尔胶-黄原胶复配胶表现出了较强的屈服应力,能在更高的压力范围内维持较高的弹性模量。随着混合温度升高,复配胶的弹性模量逐渐增大,并且在60℃时达到最大值。研究说明,普鲁兰酶改性瓜尔胶与黄原胶复配具有显著的协同增效效应。     

生物可降解聚酯PBS的合成工艺研究

目的:为了提高1,4-丁二醇的附加值和开发新型的生物可降解材料.方法:以钛酸四丁酯为催化剂通过酯化缩聚合成了聚丁二酸丁二醇酯(PBS).考察了醇酸摩尔比、催化剂用量、反应温度、反应时间等因素对酯化率的影响.结果:醇酸物质的量比为1∶1.2,催化剂用量为0.6%(质量百分含量),反应温度220℃,反应时间6h,酯化率可达98.7%,平均分子量和分子量分布分别为:Mn=182197,Mw/Mn=1.626406.利用红外谱(IR)、凝胶渗透色谱(GPC)对产物进行了表征确认.     

黄原胶寡糖生物活性的研究

利用黄原胶降解菌Cellulom onassp.XT11生产的黄原胶降解酶,对黄原胶进行生物降解,生产具有不同粘度/还原末端比的黄原胶寡糖,并研究了黄原胶寡糖在清除羟基自由基、植物防卫反应中激活因子活性和对植物病原菌抑制能力等方面的生物活性,结果表明黄原胶寡糖具有清除羟基自由基能力,并能激活植物防卫系统以抵御病原菌的侵染,同时对野油菜黄单孢菌也具有抑菌活性。     

微波辐射一步法合成香料富马酸二苄酯的研究

目的:在微波辐射下,以顺丁烯二酸酐和苄醇为原料,在复合催化剂对甲苯磺酸-硫脲存在下以甲苯为带水剂一步合成了富马酸二苄酯.方法:通过熔点测定和红外光谱分析对产物进行了结构表征.采用正交试验法研究了反应物的摩尔比、催化剂用量、反应温度、辐射反应时间等对产物收率的影响.结果:实验结果表明,在微波功率为700W,n(顺丁烯二酸酸酐):n(苄醇)=1:5,复合催化剂用量为总投料量的7%,甲苯20mL,一酯化、转化、二酯化的温度分别为140℃、145℃、135℃,回流分水90min的条件下,富马酸二苄酯的收率可达92.50%.结论:采用微波辐射法复合催化合成富马酸二苄酯具有操作简便、反应时间短、产物收率高等特点.     

豆甾醇与琥珀酸酐单酯化反应工艺及动力学研究

研究了甲苯为溶剂,吡啶为催化剂,豆甾醇与琥珀酸酐的酯化反应工艺和反应动力学。探讨了反应温度、催化剂吡啶用量、反应物的摩尔配比和反应时间对酯化反应结果的影响。实验结果表明:豆甾醇与琥珀酸酐的反应产物为豆甾醇琥珀酸单酯;当吡啶的体积分数为1.5%,反应物的摩尔比为1.0∶1.6,回流下反应20 h后,豆甾醇的酯化率大于97%,反应后的溶液经蒸发回收溶剂甲苯,固体产物分别经乙醇和水洗涤除杂,所得固体在60℃下真空干燥至恒重,得到的豆甾醇琥珀酸单酯的单程收率大于86%。单酯化反应满足二级不可逆反应动力学规律,反应的活化能为85 kJ/mol。     

黄原胶与丙烯酰胺接枝共聚反应的研究

以过硫酸铵为引发剂,在N2气保护下,研究了黄原胶(XG)与丙烯酰胺(AM)的接枝共聚反应.考察了单体浓度、引发剂浓度、反应温度和反应时间等因素对接枝率及接枝效率的影响,探讨了过硫酸铵引发黄原胶接枝丙烯酰胺共聚反应的基本规律.采用红外光谱(FT-IR)、X射线粉末衍射(XRD)对接枝共聚物的结构进行研究,用热重分析(TGA)法表征了产物的热性能,并初步探讨了接枝机理.     

改善吞咽功能食品增稠剂的研究

为了提供一种适合老年吞咽障碍患者使用的增稠剂,以黄原胶和罗望子胶及麦芽糊精为原料,粘度及溶解时间为指标,采用单因素实验和正交实验相结合的方法确定胶体最适的复配比例。结果表明:复配后的胶体粘度均大于单一胶体的粘度,且三种胶体复配后的溶解速度得到了显著地提高。黄原胶、罗望子胶和麦芽糊精的最适复配比例为3∶1∶30,粘度为611mPa·s,溶解时间为3min。随后通过流变仪对复配溶液的流变特性及粘度进行分析验证。最后将最适配方的增稠剂与市面上具有代表性的国内外增稠剂进行对比,表明该配方的增稠剂不仅具有成本低及速溶的优势,还能应用于医学钡餐造影。     

Enzymatic synthesis of betulinic acid ester as an anticancer agent: Optimization study

Abstract

Immobilized Candida antarctica lipase, Novozym 435, was used to catalyze the esterification reaction between betulinic acid and phthalic anhydride to synthesize 3-O-phthalyl betulinic acid in n-hexane/chloroform. Response surface methodology based on a five-level, four-variable central composite rotatable design was employed to evaluate the effects of synthesis parameters such as reaction time, reaction temperature, enzyme amount and substrate molar ratio on the yield of ester. Based on the response surface model, the optimal enzymatic synthesis conditions were predicted to be: reaction time 20.3 h, reaction temperature 53.9°C, enzyme amount 145.6 mg, betulinic acid to phthalic anhydride molar ratio 1:1.11. The predicted yield was 65.8% and the actual yield was 64.7%.     

Fmoc-Asn(Trt)-OH与Wang树脂的合成研究

研究了Fmoc-Asn(Trt)-OH与Wang树脂的酯化反应工艺。探讨了反应策略、溶剂体系、投料比、反应时间以及反应温度等条件对手工合成Fmoc-Asn(Trt)-Wang树脂反应的影响。并用微波辅助方法与常规方法进行了对比。实验结果表明了采用HBTU/HOBt/DIEA方法的连接效率最高。对反应的优化结果为:NMP/DCM体积比为1:7,体系、摩尔比为3:1,每次反应时间4 h,温度40℃。微波对本酯化反应影响不大。     

N-乙酰化反应制备水溶性壳聚糖研究

将高度脱乙酰化的壳聚糖在均相介质中进行N-乙酰化反应,制备水溶性壳聚糖。研究了制备工艺条件对脱乙酰度及水溶性的影响。结果表明,在乙酸—乙醇均相体系中进行乙酰化反应时,壳聚糖与乙酸酐的质量比为1∶0.6,反应温度控制在20℃,反应时间为8 h时,产品的脱乙酰度在50%左右,获得了水溶性良好的N-乙酰化壳聚糖。     

Guar Gum,Xanthan Gum,and HPMC Can Define Release Mechanisms and Sustain Release of Propranolol Hydrochloride

The objectives were to characterize propranolol hydrochloride-loaded matrix tablets using guar gum, xanthan gum, and hydroxypropylmethylcellulose (HPMC) as rate-retarding polymers. Tablets were prepared by wet granulation using these polymers alone and in combination, and physical properties of the granules and tablets were studied. Drug release was evaluated in simulated gastric and intestinal media. Rugged tablets with appropriate physical properties were obtained. Empirical and semi-empirical models were fit to release data to elucidate release mechanisms. Guar gum alone was unable to control drug release until a 1:3 drug/gum ratio, where the release pattern matched a Higuchi profile. Matrix tablets incorporating HPMC provided near zero-order release over 12 h and erosion was a contributing mechanism. Combinations of HPMC with guar or xanthan gum resulted in a Higuchi release profile, revealing the dominance of the high viscosity gel formed by HPMC. As the single rate-retarding polymer, xanthan gum retarded release over 24 h and the Higuchi model best fit the data. When mixed with guar gum, at 10% or 20% xanthan levels, xanthan gum was unable to control release. However, tablets containing 30% guar gum and 30% xanthan gum behaved as if xanthan gum was the sole rate-retarding gum and drug was released by Fickian diffusion. Release profiles from certain tablets match 12-h literature profiles and the 24-h profile of Inderal^® LA. The results confirm that guar gum, xanthan gum, and HPMC can be used for the successful preparation of sustained release oral propranolol hydrochoride tablets.     

Synthesis and Fungicidal Activity of Diaryl 1,1 -Dichloroethyl-phosphonates

Non-Newtonian behavior and dynamic viscoelasticity of a series of aqueous mixed solutions of xanthan and locust bean gum were measured using a rheogoniometer, and the rheological properties were analysed. A gelation occurred in the mixture at the concentration of 0.2% total gums at room temperature. The flow curves of the mixture solutions showed a yield value and approximated to plastic behavior at 50°C. The maximum dynamic modulus was obtained when the mixing ratio of xanthan to locust bean gum was 1:2, while comparable high moduli were also obtained in the mixing ratio of 1: 3 or 1:4. A mixture of deacetylated xanthan and locust bean gum showed the highest dynamic modulus, about two times that of the mixture of native or Na-form xanthan. The dynamic modulus of the mixtures decreased rapidly with increasing temperature. In contrast, the dynamic viscosity was scarcely changed during increasing temperature in the mixing ratio of 2: 1. The dynamic modulus was decreased by addition of urea (4.0 M), NaCl (0.1%) and MgCl₂. We concluded that the intermolecular interaction between xanthan and locust bean gum might occur between the side chains of the former and backbone of the latter, as in a lock-and-key effect.     

黄原胶降解菌BIT-BJ001培养条件的优化

黄原胶在采油工程中有重要的应用,但其难降解性质给采油工程带来很多问题。从塔里木油田胡杨木根部样品中分离得到1株黄原胶降解菌BIT-BJ001,对其发酵条件的研究表明,此黄原胶降解菌最适培养条件为:黄原胶0.3%,酵母粉0.5%,Na+浓度0.8%,Mg2+浓度0.8%,初始pH值为10,温度60℃。菌种BIT-BJ001降解黄原胶的能力与发酵时间、发酵液中还原糖浓度有关,发酵96 h,黄原胶降粘率达到最高,发酵液中还原糖浓度过高,将抑制菌株对黄原胶的降解。     

Novozyme 435-Catalyzed Asymmetric Acylation of (R,S)-3-n-Butylphthalide in Hexane

Abstract

The asymmetric acylation of (R, S)-3-n-butylphthalide could be efficiently catalyzed by Novozyme 435. The effect of various reaction parameters such as water activity, temperature, molar ratio of acetic anhydride to (R, S)-3-n-butylphthalide, and reaction time on the asymmetric acylation were studied. The optimums of the reaction parameters were water activity 0.62, temperature 30°C, molar ratio of acetic anhydride to (R, S)-3-n-butylphthalide 8:1, and reaction time 48 h, respectively. Under the optimum conditions, enantiopure 3-n-butylphthalide with an optical purity of 95.7% enantiomeric excess and 49.1% yield could be obtained. Furthermore, the enantiomeric excess of product was over 98%.     

Chemical modification of Cassia occidentalis seed gum: carbamoylethylation

The seeds of Cassia occidentalis, an annual weed occurring throughout India, is a rich source of galactomannan gum. The gum derived from seed endosperm can be potentially utilized in a number of industries to replace the conventional gums. With a view to utilize the gum for broader applications, carbamoylethylation of C. occidentalis seed gum was carried out with acrylamide in presence of sodium hydroxide under different reaction conditions. Variables studied were concentration of sodium hydroxide, acrylamide, gum–solvent ratio, reaction time and temperature. The nitrogen content, carboxyl content and total ether content were determined. The optimum condition for preparing carbamoylethyl C. occidentalis seed gum (%N=2.57) comprised concentration of acrylamide (0.070 mol), sodium hydroxide (0.125 mol), C. occidentalis seed gum (0.03 mol) at 30 °C for 3 h. Rheological properties of carbamoylethyl C. occidentalis seed gum solution showed non-Newtonian pseudo-plastic behavior, relatively high viscosity, cold water solubility and solution clarity vis-à-vis unmodified C. occidentalis seed gum.     

Synergistic interaction between xanthan and guar gum

The non-Newtonian behavior and dynamic viscoelasticity of a series of aqueous mixtures of xanthan and guar gum were measured with a rheogoniometer. At a concentration of 0.2% of total gums, gelation did not occur at room temperature but occurred at a low temperature (0°). A much stronger interaction was observed with a mixture of deacetylated xanthan than that with native xanthan. The maximum dynamic modulus was obtained when the ratio of xanthan to guar gum was 2:1. The transition temperatures of dynamic viscoelasticity for mixtures with native and deacetylated xanthan were observed at 25 and 30°, respectively. It was concluded that the side chains of the guar gum molecular prevent an intermolecular interaction with the side chains of the xanthan molecule. An intermolecular interaction between xanthan and guar gum at low temperature might be promoted between the periphery of the side chains of the xanthan molecule and the backbone of the guar gum molecule and dissociation takes place at the transition temperature.