气相色谱法测定鱼油多烯乙酯的含量

目的用气相色谱法测定鱼油多烯乙酯中二十碳五烯酸乙酯 (EPA E)和二十二碳六烯酸乙酯 (DHA E)的含量。方法采用气相色谱法 ,聚二乙二醇酯为固定相 ,涂布浓度为 10 % ,载体为ChromosorbWAWDMCS 80～ 10 0目的气相柱。结果EPA E平均回收率为 10 0 .31% ,RSD为 2 .5 4 % ;DHA E平均回收率为 10 3.37% ,RSD为 2 .76 %。结论此法操作简便、准确、重现性、稳定性好 ,是一种可行的含量测定方法     

中国淡水鱼油的研究 Ⅱn-3多不饱和脂肪酸乙酯的制备及浓缩工艺探讨

对从淡水鱼的下脚料中制备及浓缩n-3多不饱和脂肪酸乙酯进行了工艺探讨。依次采取冷冻、结晶法、减压蒸馏法和尿素包合物吸附法,使得淡水鱼油的n-3多不饱和脂肪酸乙酯的含量≥65％,其中二十碳五烯酸(eicosapentaenoic acid,EPA)乙酯和二十二碳六烯酸(docosahexaenoic acid,DHA)乙酯总量≥30％。     

毛细管气相色谱法测定邻苯二甲酸二乙酯中16种邻苯二甲酸酯类杂质含量

目的:建立邻苯二甲酸二乙酯中16种邻苯二甲酸酯类杂质的测定方法。方法 :采用毛细管气相色谱法,以(5%)苯基-(95%)甲基聚硅氧烷为固定液,柱温为150℃,保持1 min,以10℃.min-1升温至220℃,再以5℃.min-1升温至300℃,保持6 min;进样口温度为250℃;检测器温度为350℃;载气流量为1℃.min-1;进样量1μL,分流比10:1。以邻苯二甲酸二乙酯为对照品,按标准曲线法以峰面积计算邻苯二甲酸二乙酯中16种邻苯二甲酸酯类杂质的含量。结果 :在选定的色谱条件下,邻苯二甲酸二乙酯与16种邻苯二甲酸酯类杂质分离良好,邻苯二甲酸二乙酯在12.6～126μg.mL-1的范围内线性关系良好,回归方程为Y=0.0271X+0.0007(r=1);16种邻苯二甲酸酯类杂质邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二异丁酯(DIBP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2-甲氧基)乙酯(DMEP)、邻苯二甲酸二(4-甲基-2-戊基)酯(BMPP)、邻苯二甲酸二(2-乙氧基)乙酯(DEEP)、邻苯二甲酸二戊酯(DPP)、邻苯二甲酸二己酯(DHP)、邻苯二甲酸丁苄酯(BBP)、邻苯二甲酸二(2-丁氧基)乙酯(DBEP)、邻苯二甲酸二环己酯(DCHP)、邻苯二甲酸二辛酯(DEHP)、邻苯二甲酸二苯酯、邻苯二甲酸二正辛酯(DNOP)、邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二壬酯(DNP)检出限均在0.25μg.mL-1以下;精密度RSD均在2.0%以下;平均回收率均在82.3%～105.4%范围内。结论:该方法准确、可靠,可用于邻苯二甲酸二乙酯中16种邻苯二甲酸酯类杂质的检测。     

阿魏酸乙酯的药理活性及其机制研究

目的 :观察阿魏酸乙酯的药理活性及其机制。方法 :在兔富含血小板血浆 (PRP)中加入阿魏酸乙酯和阿魏酸 ,用ADP诱导血小板的集聚 ,用TYXN 91智能血液凝集仪观察血小板聚集率 ,激光共聚焦显微镜观察血小板细胞聚集时细胞内钙离子的变化情况。制备CCl4肝损伤小鼠模型 ,取血清测定谷丙转氨酶 (ALT)、谷草转氨酶 (AST)活性 ,取肝组织测定丙二醛 (MDA)水平及超氧化物歧化酶 (SOD)活性。结果 :不同浓度的阿魏酸乙酯 ,对ADP诱导的血小板聚集抑制百分数均显著高于等浓度的阿魏酸(n =8,P <0 .0 5 )。在阿魏酸乙酯作用下ADP诱导的血小板细胞内钙离子荧光强度的变化 (ΔFI)为4 .6± 1.7,明显低于对照组ΔFI值 (10 .3± 2 .6 ,n =8,P <0 .0 1)。阿魏酸乙酯可使肝损伤小鼠组织MDA、血清ALT、AST含量显著低于对照组 ,而肝组织的SOD水平显著高于对照组。结论 :阿魏酸乙酯抑制ADP诱导的血小板聚集作用及对CCl4引起的小鼠急性肝损伤的保护作用均比阿魏酸强。     

苯磺酸氨氯地平原料中基因毒性杂质苯磺酸甲酯与苯磺酸乙酯的含量测定

目的:建立苯磺酸氨氯地平原料中基因毒性杂质苯磺酸甲酯与苯磺酸乙酯含量的高效液相色谱法(HPLC)测定方法。方法:采用Welch Ultimate Plus-C18(Ⅱ)色谱柱(250 mm×4.6 mm,5μm),以磷酸三乙胺缓冲液(pH=3.0)-乙腈为流动相梯度洗脱,检测波长为220 nm,流速为1.0 mL/min,柱温为30℃,研究苯磺酸氨氯地平原料中基因毒性杂质苯磺酸甲酯与苯磺酸乙酯定量测定。结果:苯磺酸甲酯和苯磺酸乙酯吸收峰与氨氯地平能达到有效分离;苯磺酸甲酯浓度在0.102 9～1.633 9μg/mL范围内呈良好线性关系(r=0.999 8),平均回收率为103.6%;苯磺酸乙酯浓度在0.103 3～1.656 1μg/mL范围内呈良好线性关系(r=0.999 8),平均回收率为102.7%;共检测6批苯磺酸氨氯地平原料,且均未检测出苯磺酸甲酯与苯磺酸乙酯的量。结论:本法专属性强,准确度与重复性良好,可用于苯磺酸氨氯地平原料中基因毒性杂质苯磺酸甲酯与苯磺酸乙酯的控制。     

丙酮酸乙酯对胶原诱导性关节炎大鼠血清肿瘤坏死因子-α白细胞介素-17转化生长因子-β_1的影响

目的观察丙酮酸乙酯对胶原诱导性关节炎(CIA)大鼠血清肿瘤坏死因子(TNF)-α,白细胞介素(IL)-17和转化生长因子(TGF)-β1的影响,探讨其用于治疗类风湿关节炎的可能性。方法实验大鼠分为正常对照组、CIA对照组及丙酮酸乙酯治疗组,建立大鼠CIA动物模型,记录大鼠的一般情况,目测评分其关节炎指数,ELISA法检测血清TNF-α,IL-17和TGF-β1浓度。结果①丙酮酸乙酯治疗组大鼠平均体质量高于CIA对照组,关节炎指数低于CIA对照组(P<0.05);②丙酮酸乙酯治疗组大鼠血清TNF-α和IL-17水平较CIA对照组明显降低,TGF-β1水平明显升高(P<0.05)。结论丙酮酸乙酯能明显改善CIA大鼠的生存状态,减轻其关节肿胀,显著降低大鼠血清中TNF-α和IL-17水平,提高TGF-β1水平,有可能成为治疗类风湿关节炎的新药物。     

乙氧甲叉丙二酸二乙酯制备方法的改进

乙氧甲叉丙二酸二乙酯是由丙二酸二乙酯和原甲酸三乙酯在乙酸酐和氯化锌催化下缩合而成的,收率97.3％(以丙二酸二乙酯计算)。原甲酸三乙酯的投料量是过量的,没反应的原甲酸三乙酯回收后套用在下一釜反应中。     

氯氟乙酯(25例)和地西泮(23例)治疗焦虑障碍的疗效和安全性比较

目的 :评价氯氟乙酯治疗焦虑障碍的疗效和安全性。方法 :采用双盲、双模拟、随机、平行对照研究。完成 4wk治疗的病人共 4 8例。其中试验组 (氯氟乙酯组 ) 2 5例 ,对照组 (地西泮组 ) 2 3例。试验组早、午餐后服氯氟乙酯安慰剂及地西泮安慰剂各 1片 ,晚餐后服氯氟乙酯 2mg及地西泮安慰剂各 1片 ;对照组早、午、晚餐后服氯氟乙酯安慰剂及地西泮 2 .5mg各 1片 ,疗程为 4wk。结果 :治疗 4wk后 ,试验组的HAMA总分显著降低 ,HAMA减分率达 (5 9± 2 5 ) % ,临床总有效率达72 % ,与对照组相比无显著意义 (P >0 .0 5 )。试验组的不良反应的发生率为 8% ,与对照组相比无显著意义 (P >0 .0 5 )。结论 :氯氟乙酯治疗焦虑障碍的疗效 ,与地西泮相似 ,无明显不良反应。     

紫外分光光度法测定芳香维甲酸乙酯胶囊的含量

目的:测定芳香维甲酸乙酯胶囊中芳香维甲酸乙酯的含量.方法:采用紫外分光光度法,测定波长为(306±1)nm.结果:芳香维甲酸乙酯浓度在2～12 μg/m1范围内与吸收度的线性关系良好,标准曲线回归方程为A=0.068 93 C-0.005 333,r=0.999 9,平均回收率为99.9%,RSD=0.74%.结论:紫外分光光度法简便,测定结果准确、重现性好,可用于芳香维甲酸乙酯的质量控制.     

大口径毛细管柱气相色谱法测定鱼油软胶囊中EPA-E和DHA-E的含量

目的 测定鱼油软胶囊中二十碳五烯酸乙酯(EPA-E)和二十二碳六烯酸乙酯(DHA-E)的含量。方法采用530μm大口径毛细管柱气相色谱法,外标法测定EPA-E和DHA-E的含量。结果EPA-E和DHA-E的保留时间分别为8．0min和12．0min,其标准曲线分别在0．52～1．22μg和0．58～1．36μg之间有良好的线性关系,回收率分别为97．1％和98．2％。结论该方法专属性强,适用于鱼油软胶囊中EPA-E和DHA-E的定量分析。     

Designing of antiepileptic ligands by esterification and acetylation of dipeptides

Glycylglycine, alanylalanine and alanylglycine were synthesized, their free carboxylic and amino groups were converted to methyl esters of N-acetylglycylglycine, N-acetylalanylglycine and N-acetylalanylalanine. The synthesized compounds were evaluated for antiepileptic activity, plasmaprotein binding, TD₅₀ and potentiating effect of phenobarbitone sodium.     

RP-HPLC法测定布洛芬丁香酚酯微乳中布洛芬丁香酚酯及有关物质含量

目的测定布洛芬丁香酚酯(ibuprofen eugenol ester,IEE)微乳中布洛芬丁香酚酯及有关物质的含量。方法微乳用甲醇溶解,采用RP HPLC法。色谱柱:ODS色谱柱;流动相:甲醇体积分数为0.2%的三氟乙酸四氢呋喃(体积比为170∶20∶15);流速:1.0 mL.min-1;检测波长:230 nm;室温测定。结果RP HPLC法测定的线性范围为0.5~50 mg.L-1,相关系数r=0.999 8;微乳中布洛芬酯的平均回收率为99.95%(RSD=0.35%,n=9);最低检测限50 ng;重复性良好(RSD=0.71%)。结论该方法适用于布洛芬丁香酚酯及有关物质的含量测定。     

Two pairs of unusual melibiose and raffinose esters from Scrophularia ningpoensis

A pair of unusual melibiose esters (1α/1β) and a pair of unusual raffinose esters (2α/2β), were isolated from Scrophularia ningpoensis. Structures of them were established by detailed spectroscopic analyses to be 6-O-(E)-cinnamoyl-α-d-galactopyranosyl-(1→6)-α(β)-d-glucopyranose (1α/1β) and 6-O-(E)/(Z)-cinnamoyl-α-d-galactopyranosyl-(1→6)-α-d-glucopyranosyl-(1→2)-β-d-fructofuranose (2α/2β), respectively. All these compounds were evaluated for antifouling activity against the settlement of Balanus amphitrite larvae, along with the cytotoxic effect against the proliferation of HeLa cell lines.     

Similar effects of succinic acid dimethyl ester and glucose on islet calcium oscillations and insulin release

The relative contribution of glycolysis vs. oxidative metabolism to the stimulus secretion coupling mechanism of beta-cells was investigated in isolated islets. For that purpose, the secretory and intracellular calcium responses of islets to both glucose and succinic acid dimethyl ester (SAD) were compared. After 45 min of rat islet perifusion in the absence of substrates, the maximum secretory responses to glucose (20 mmol/L) and SAD (10 mmol/L) were qualitatively and quantitatively indistinguishable. Malonic acid dimethyl ester (a permeable citric acid cycle inhibitor) suppressed the insulin secretory response to both 20 mmol/L glucose and 10 mmol/L SAD (-70% on average). The inhibitor decreased within 70% the rate of 14CO2-production from 10 mmol/L [2-(14)C]pyruvate without affecting the rate of 20 mmol/L D-[5-(3)H]glucose utilization. Both, 11.1 mmol/L glucose and 10 mmol/L SAD, elevated the intracellular calcium concentration and induced a similar pattern of oscillations that were rapidly ablated by 20 mmol/L malonic acid dimethyl ester. However, the intracellular concentration of calcium declined to basal values several minutes after the introduction of the inhibitor in the presence of SAD whereas it remained elevated in the case of glucose. In conclusion: (1) An exclusive increase of mitochondrial metabolism in pancreatic islets was sufficient to mimic the effects of glucose on intracellular calcium and insulin secretion. (2) Islet glycolysis and/or the re-oxidation of cytoplasmic NADH allowed the maintenance of an elevated, though non-oscillating, intracellular calcium concentration, but a reduced response to glucose.     

Depressor effects of isoguvacine propyl ester and isoarecaidine propyl ester due to stimulation of central GABA receptors in the cat

Upon their simultaneous administration into the left and right vertebral artery of the cat, 2 × 30 μg isoarecaidine propyl ester (IAPE) and 2 × 30 μg isoguvacine propyl ester (IGPE) induce hypotension and bradycardia. These effects were antagonized by (+)-bicuculline or picrotoxin. IAPE is rapidly hydrolyzed by cat brain tissue in vivo. It is suggested that both IAPE and IGPE are prodrugs and that the corresponding carboxylic acids are GABA agonists and responsible for the cardiovascular effects evoked.     

阿司匹林丁醇酯的合成

目的合成前药阿司匹林丁醇酯。方法以水杨酸为原料,用乙酸酐酰化得到阿司匹林,然后以DCC为脱水剂,与丁醇缩合得到阿司匹林丁醇酯。结果合成了阿司匹林丁醇酯。结论目标化合物的结构经IR、1H NMR确证。     

Tenuifoliose Q, a new oligosaccharide ester from the root of Polygala tenuifolia Willd

From the cortexes of Polygala tenuifolia Willd., a new oligosaccharide ester, tenuifoliose Q (1), was isolated together with three known compounds. The structure of 1 was elucidated by spectroscopic and physiochemical analysis as an oligosaccharide esterified with acetic, benzoic and p-hydroxycinnamoyl acid.     

改变原料配比提高头孢曲松钠收率

目的：提高头孢曲松钠收率。方法：调整原料配比,减少原料消耗提高头孢曲松钠收率。结果：根据实验原料AE活性酯对收率的影响很明显。结论：减少AE活性酯的投入量可以使收率稳定。     

Tenuifoliose Q,a new oligosaccharide ester from the root of Polygala tenuifolia willd.

From the cortexes of Polygala tenuifolia Willd., a new oligosaccharide ester, tenuifoliose Q (1), was isolated together with three known compounds. The structure of 1 was elucidated by spectroscopic and physiochemical analysis as an oligosaccharide esterified with acetic, benzoic and p-hydroxycinnamoyl acid.     

Some equilibrium and kinetic aspects of water sorption in poly(ortho ester) s

Poly(ortho ester)s are a class of erodible polymers suitable for the construction of drug delivery systems. Since the release of bioactive substances from these polymers depends on the hydrolytic cleavage of the backbone, the isothermal sorption and transport of water in various poly(ortho ester)s have been investigated. At 25°C and relative vapor pressure equal to unity, the amount of water sorbed at saturation ranges from 0.3% to 0.75% w/w. Application of a modified Henry's law to the data yields reasonable correlation. The diffusion coefficient of water in poly(ortho ester)s appears to be independent of film thickness, molecular weight and water activity. At experimental temperatures above the glass transition temperature of the polymers, a marked increase in water diffusivity was observed. The activation energies of the transport process are within the range usually found for synthetic polymers. These equilibrium and kinetic studies suggest that membranes made of copolymers tend to have a more open structure than single diol poly(ortho ester)s.