薄层色谱法检查熊去氧胆酸的有关物质

目的:建立熊去氧胆酸有关物质检查的薄层色谱方法。方法:以丙酮-水(9∶1)为溶剂,制备熊去氧胆酸溶液(10 mg.mL-1),鹅去氧胆酸对照溶液+熊去氧胆酸对照溶液(各0.4 mg.mL-1)、鹅去氧胆酸对照溶液(0.1 mg.mL-1)、胆石酸对照溶液(0.01 mg.mL-1)、胆酸对照溶液(0.05 mg.mL-1)、系列自身对照溶液(0.01,0.02,0.05 mg.mL-1);各点样5μL于硅胶G薄层板上,以二氯甲烷-丙酮-冰醋酸(60∶30∶3)为展开剂,以4.5%磷钼酸硫酸溶液-冰醋酸(1∶20)溶液为显色剂。结果:熊去氧胆酸与鹅去氧胆酸分离较好;熊去氧胆酸可能含有的各有关物质的斑点清晰可见。结论:本法适用于熊去氧胆酸的质量控制。     

RP-HPLC法测定熊去氧胆酸胶囊中熊去氧胆酸及有关物质的含量

目的建立反相高效液相色谱法(RP-HPLC)测定熊去氧胆酸胶囊中熊去氧胆酸、胆酸、鹅去氧胆酸及胆石酸的含量。方法使用Diamonsil C18色谱柱(200 mm×4.6 mm,5μm),流动相为乙腈-0.03 mol·L-1磷酸溶液(体积比为40∶60),流速为1.4 mL·min-1,检测波长为205 nm,柱温为35℃。结果熊去氧胆酸胶囊中熊去氧胆酸、胆酸、鹅去氧胆酸及胆石酸在25 min内洗脱并基线分离。熊去氧胆酸、胆酸、鹅去氧胆酸及胆石酸的线性范围分别为0.80²00.00、0.45200.00、0.45¹10.00、0.30110.00、0.30⁷0.00和0.3070.00和0.30⁸0.00 mg·L-1,平均回收率分别为99.7%、99.3%、98.7%和99.1%,RSD分别为1.30%、1.47%、1.87%和1.95%(n=3)。结论 RP-HPLC可用于同时测定熊去氧胆酸胶囊中熊去氧胆酸、胆酸、鹅去氧胆酸及胆石酸的含量,可应用于熊去氧胆酸胶囊胶囊制剂的质量控制。     

RP—HPLC法测定熊去氧胆酸中的有关物质

目的:建立HPLC外标法同时测定熊去氧胆酸中4种特殊杂质及其他有关物质含量。方法:采用Luna C_(18)柱(150mm×4.6mm,5μm),以乙腈-0.001mol·L~(-1)磷酸二氢钠溶液(45∶55,用磷酸调pH至2.2±0.1)为流动相,流速为1.0mL·min~(-1),柱温为30℃,检测波长206nm。结果:熊去氧胆酸、胆酸、胆石酸、鹅去氧胆酸、7-酮基胆石酸分别在0.1～2.0,0.04～1.2,0.5～10,0.08～1.6,0.072～0.72mg·mL~(-1)范围内线性关系良好(r≥0.9998);方法的精密度和重复性良好(RSD<2%)。结论:该方法准确、简便、快速,适用于熊去氧胆酸的质量控制。     

HPLC法测定熊去氧胆酸片有关物质的含量

[摘要]目的：建立高效液相色谱法测定熊去氧胆酸片有关物质含量的方法。方法：用十八烷基硅烷键合硅胶为填充剂，以磷酸盐缓冲液（pH3.0）-甲醇-乙腈（35:37:28）为流动相，示差折光检测器测定。结果：在选定的色谱条件下，各成分可达到很好的分离，7-酮基胆石酸、胆酸、鹅去氧胆酸、胆石酸分别在0.05~2.00，0.05~2.00，0.05~2.00，0.10~2.00mg·mL-1的范围内线性关系良好(r>0.9989)；精密度、稳定性试验的RSD均不大于0.5%；回收率分别为100.1%、99.8%、100.7%和101.9%（n=9,RSD<1.4%）。7-酮基胆石酸、胆酸、鹅去氧胆酸、胆石酸定量限分别为3.0、2.5、7.0、20μg·mL-1，检测限分别为0.8、0.7、2.0、3.5μg·mL-1。测定供试品两批，供试品一7-酮基胆石酸检出量为0.03%，胆酸和胆石酸均未检出，鹅去氧胆酸检出量为0.66%；供试品二7-酮基胆石酸、鹅去氧胆酸检出量均为0.10%，胆酸和胆石酸均未检出。结论：该方法灵敏度高，专属性强，适于测定熊去氧胆酸片中有关物质的含量。     

小儿氨酚黄那敏颗粒中人工牛黄鉴别方法的改进

目的对小儿氨酚黄那敏颗粒中人工牛黄的鉴别方法进行研究。方法采用硅胶G薄层板,分别以异辛烷-乙酸丁酯-冰醋酸-甲酸(8∶10∶5∶1)为展开剂,制定了人工牛黄中的胆酸、猪去氧胆酸的薄层色谱鉴别。结果色谱斑点清晰,重现性好。结论该方法操作简便,专属性强。     

口服胆结石溶解剂

本品以熊去胆酸和L-薄荷醇为活性成舒。其中熊去氧胆酸为微晶粉,其重量比为80-20％(最好为50％),L-薄荷醇为20-80％(最好为50％),将上述活性成分包于软胶囊中。此混合物有协同作用,能增加胆石的溶解速率,减少熊去氧胆酸的用量为原来     

高效液相色谱法测定荷胆胶囊中牛磺熊去氧胆酸含量

目的建立测定荷胆胶囊中牛磺熊去氧胆酸含量的高效液相色谱法。方法采用Alltech Alltima C18色谱柱(250 mm×4.6 mm,5μm),流动相为用磷酸调pH至4.4的甲醇-0.03 mol/L磷酸二氢钠溶液(65∶35),流速1 mL/min,检测波长210 nm。结果牛磺熊去氧胆酸进样量在4.067 4～12.2μg范围内与峰面积线性关系良好(r=0.999 6),平均回收率为97.99%,RSD=1.43%(n=6)。结论高效液相色谱法快速、准确、有效,可用于荷胆胶囊中牛磺熊去氧胆酸的含量测定。     

HPLC测定牛磺熊去氧胆酸胶囊中的有关物质

目的采用RP-HPLC法测定牛磺熊去氧胆酸胶囊中的有关物质。方法采用Diamonsil C18色谱柱(150 mm×4.6mm,5μm),流动相为0.02 mol.L-1磷酸二氢钠-乙腈(60∶40,磷酸调pH5.5),检测波长为205 nm,流速为1.0 mL.min-1,柱温30℃。结果牛磺熊去氧胆酸0.9694～96.94μg.mL-1与峰面积的线性关系良好(r=0.9999),检测限为0.3635 ng,定量限为1.454 ng。牛磺鹅去氧胆酸0.9443～94.43μg.mL-1与峰面积的线性关系良好(r=0.9999),检测限为9.447 ng,定量限为23.62 ng,方法回收率为99.54%。结论所用方法准确、灵敏、快速,适用于牛磺熊去氧胆酸胶囊中微量杂质的控制。     

鹅去氧胆酸的纯化

鹅去氧胆酸(chenodeoxycholic acid;CDCA),化学名:3α,7α-二羟基-5β-胆烷酸,为七十年代开发的胆石溶解剂,也是合成熊去氧胆酸(urso deoxycholic acid;UDCA)的原料。其制备可直接从禽胆汁提取,或用脱氢胆酸生物转化成二羟基-12-氧代胆烷酸,然后用黄鸣龙法还原;但以胆酸为起始原料的半合成法,工艺成熟,适合于生产条件。     

治疗胆石症的新药——鹅去氧胆酸

最近,国外正在研究一种治疗胆石症的新药,名为鹅去氧胆酸(Chenodeoxycholicacid),给胆固醇胆石症患者服用后,能使胆石渐渐溶解,这样就不必进行外科手术。鹅去氧胆酸是一种天然的胆酸,以和甘氨酸或牛磺氨酸相结合的形式,存在于人、牛、猪及鹅、鸡等家禽胆汁中,在人胆汁中占45％,为最多的一种胆汁酸。其化学名为3α,7α-二羟基-5β-胆烷酸,为无味、无色的针状结晶(醋酸乙酯中重结晶),可溶于甲醇、乙醇、丙酮、冰醋酸,不溶于水、石油醚、苯。其结构式为     

甘露醇-旋光法测定鞣柳硼三酸散中硼酸的含量

目的建立旋光法测定鞣柳硼三酸散中硼酸的含量。方法以低浓度明胶溶液提取制剂中硼酸,利用甘露醇结合硼酸形成具有旋光性复合物,并建立鞣柳硼三酸散中硼酸的含量测定方法。结果硼酸浓度在5～20 g.L-1的浓度范围内与旋光度线性关系良好(r=0.999 2),方法的平均回收率为99.98%,RSD为1.3%。结论旋光法测定鞣柳硼三酸散中硼酸的含量,操作简便、快速,结果准确,重现性好。     

咖啡酸、阿魏酸和香草酸对酪氨酸酶活性的影响

目的 :研究咖啡酸、阿魏酸和香草酸对酪氨酸酶活性的影响 ,寻找酪氨酸酶抑制剂 ,从而为治疗色素增加性皮肤病筛选药物。方法 :酪氨酸酶多巴速率氧化法体外测定药物干预前后酪氨酸酶活性 ,求出酪氨酸酶抑制率。采用Lineweaver Burk双倒数法制得酶动力学曲线 ,推断抑制类型。结果 :3种试药中仅香草酸对酪氨酸酶具有抑制作用 ,与氢醌比较无显著差异 (P >0 .0 5 ) ,咖啡酸、阿魏酸对酪氨酸酶具有上调激活作用。结论 :香草酸为良好的混合型酪氨酸酶抑制剂。     

Nalidixic acid prodrugs: Amides from amino acid ester and nalidixic acid

Amides from amino acid ester and nalidixic acid were synthesized. The solubility characteristics and partition coefficient of the compounds were studied. The hydrolysis of the compounds was studied in the simulated gastric fluid and simulated intestinal fluid. Some compounds showed better antibacterial activity than nalidixic acid.     

Oral antipyretic therapy: Evaluation of the N-aryl-anthranilic acid derivatives mefenamic acid,tolfenamic acid and flufenamic acid

Summary The antipyretic activity of three N-aryl-anthranilic acid derivatives, mefenamic acid, tolfenamic acid and flufenamic acid, was compared and their optimal antipyretic dose determined in a trial in 87 children (aged 5 months to 15 years), who suffered from infections and fever exceeding 38.5°C. Tolfenamic acid proved to be the most potent antipyretic agent of the three drugs; it was eight times more powerful than mefenamic acid and three times more powerful than flufenamic acid. The optimal antipyretic doses were: mefenamic acid 4 mg/kg, tolfenamic acid 0.5 mg/kg and flufenamic acid 1.5 mg/kg. It is evident that the antipyretic activity of these anthranilic acid derivatives is even greater than their antirheumatic effect, the difference being most noticeable in the case of tolfenamic acid.     

高效液相色谱法测定鞣柳硼三酸散中水杨酸的含量

目的:探讨用反相高效液相色谱法测定鞣柳硼三酸散中水杨酸的含量。方法:采用Symetry Shield RP18(5μm 4.6mm×250mm)Columm色谱柱;以0.05mol/L磷酸二氢钠缓冲液(pH2.6)-乙腈(50∶50)为流动相;检测波长233nm。结果:水杨酸在20.4～61.2μg/ml浓度范围内呈良好的线性关系,平均回收率为99.0%。结论:本法简便、准确、快速,适用于鞣柳硼三酸散中水杨酸的含量测定。     

高效液相色谱法测定复方苯甲酸乳膏中苯甲酸和水杨酸的含量

目的:建立高效液相色谱法(HPLC)测定复方苯甲酸乳膏中苯甲酸和水杨酸的含量。方法:色谱柱为Hypersil C_(18)柱(4.6nm×250mm,5μm),流动相为甲醇-水(44:56),流速0.8mL·min~(-1),检测波长为226nm。结果:苯甲酸和水杨酸分别在15.20～76.00mg·L~(-1)和7.64～38.20mg·L~(-1)范围内线性良好(r=0.9999);日内、日间RSD在0.030～4.79％,高、中、低浓度回收率在98.54％～101.20％。分析了3批样品,结果满意。结论:本方法简便,快速,准确,可作为复方苯甲酸乳膏的质量控制方法。     

双波长薄层扫描法测定苯甲酸复方制剂的含量

本文采用硅胶HF_(254 366)薄层板,以氯仿—丙酮—异丙醇—甲醇—浓氨水(30:30:15:15:10)为展开剂,直接分离苯甲酸复方制剂中的苯甲酸与水杨酸。在CS-930型双波长薄层扫描仪上,采用反射式锯齿扫描,分别对苯甲酸和水杨酸进行扫描测定。结果:苯甲酸与水杨酸的线性关系、精度及回收率都比较满意。     

Methylated eicosapentaenoic acid and tetradecylthioacetic acid: effects on fatty acid metabolism.

We introduced methyl or ethyl groups to the 2- or 3-position of the eicosapentaenoic acid (EPA) molecule to investigate whether the branching of EPA could influence its hypolipidemic effect in rats. The most effective branching involved two methyl groups in the 2-position and one methyl group in the 3-position. These EPA derivatives increased hepatic mitochondrial and peroxisomal beta-oxidation and decreased plasma lipids concomitant with suppressed acetyl-coenzyme A (CoA) carboxylase (EC 6.4.1.2) and fatty acid synthase (EC 2.3.1.85) activities. This was followed by elevated activities of camitine O-palmitoyltransferase (EC 2.3.1.21) and possibly 2,4-dienoyl-CoA reductase (EC 1.3.1.34), as well as induced mRNA levels of these enzymes and fatty acyl-CoA oxidase. The fatty acid composition in liver changed, with an increased 18:1 n-9 content, whereas the expression of delta9-desaturase remained unchanged. We investigated the flux of fatty acids in cultured hepatocytes, and found that oxidation of [1-14C]-labeled palmitic acid increased but the secretion of palmitic acid-labeled triglycerides decreased after addition of 2-methyl-EPA. The fatty acyl-CoA oxidase (EC 1.3.3.6) activity in these cells remained unchanged. A significant negative correlation was obtained between palmitic acid oxidation and palmitic acid-labeled synthesized triglycerides. To investigate whether the hypolipidemic effect occurred independently of induced peroxisomal beta-oxidation, we fed rats 2-methyl-tetradecylthioacetic acid. This compound increased the peroxisomal but not the mitochondrial beta-oxidation, and the plasma lipid levels were unchanged. In conclusion, EPA methylated in the 2- or 3-position renders it more potent as a hypolipidemic agent. Furthermore, this study supports the hypothesis that the mitochondrion is the primary site for the hypolipidemic effect.