不同提取方法对人工牛黄中胆酸含量的影响

目的:研究不同提取方法对人工牛黄中胆酸含量的影响。方法:选择3个不同产地的人工牛黄,采用经水解处理和未经水解处理2种方法提取胆酸,并用高效液相色谱-蒸发光散射检测法测定胆酸含量。结果:经水解处理的样品中胆酸含量高于未经水解处理的同批样品。结论:水解过程将人工牛黄中的结合型胆酸转化为游离型胆酸,从而使胆酸的含量升高。因此,将总胆酸含量和游离胆酸含量共同作为人工牛黄质量控制的指标更为合理。     

HPLC-ELSD法测定清开灵注射液中胆酸和猪去氧胆酸的含量

目的：采用高效液相色谱蒸发光散射检测器测定清开灵注射液中胆酸和猪去氧胆酸的含量。方法：采用CLC-ODS柱，以甲醇-水-冰醋酸（80：20：0．01）为流动相，蒸发光散射检测器。结果：胆酸及猪去氧胆酸分勇1在1.604～8.020μg、1.068～5．340μg线性关系良好；胆酸及猪去氧胆酸的平均回收率分别为97．4％、99．2％。结论：该方法简便、准确、分离效果好；本方法可用于清开灵注射液的质量评价。     

HPLC-ELSD法测定黄栀巴布贴中胆酸的含量

目的：建立测定黄栀巴布贴中胆酸含量的检测方法。方法：采用高效液相法蒸发光散射检测器（HPLC-ELSD）测定,色谱条件为：KromasilC18（250mm×4．6mm,5μm）;流动相为甲醇-乙腈-2％醋酸溶液（60：10：30）;蒸发光散射检测器检测参数：漂移管温度75oC,栽气（N2）流速2．0ml·min-1。结果：胆酸在0．098—1．960μg（r：0．9991）范围内线性关系良好,平均加样回收率为97．7％,RSD为1．5％。结论：该法操作简便,结果准确,重复性好,可以控制黄栀巴布贴的含量。     

HPLC—ELSD测定克拉霉素胶囊的含量

目的研究克拉霉素胶囊的含量测定方法。方法用高效液相色谱．蒸发光散射检测法进行含量测定。结果该方法能很好分离被测组分与其他杂质,在实验浓度范围内峰面积的对数值与浓度的对数值呈良好的线性关系,r=0．9998,RSD=0．36％。结论用高效液相色谱-蒸发光散射检测法测定克拉霉素胶囊的含量,方法简便,结果准确。     

高效液相色谱-蒸发光散射检测器分析雷帕霉素

雷帕霉素在国内属二类新药 ,由于雷帕霉素在溶液中存在互变异构现象 ,使得分离、分析变得较为复杂。本文在查阅文献的基础上建立了蒸发光散射检测器 (ＥＬＳＤ)的检测方法 ,对雷帕霉素、异构体及有关物质进行了考察。1　材料与方法高效液相色谱仪 :Ｗａｔｅｒｓ 2 6 90＆996色谱系统 ;ＨＰ110 0色谱仪 ;ＨＰ110 0紫外检测器 ;ＨＰ110 0色谱工作站 ;Ａｌｌ ｔｅｃｈ2 0 0 0蒸发光散射检测器 ;江申色谱工作站。蒸发光散射检测器与紫外检测器为串联使用。雷帕霉素由华北制药厂提供 ,批号 :130 5 2 1- 2 0 0 0 0 1Ｗ ;正己烷、氯丁烷、乙腈、甲…     

高效液相色谱-蒸发光散射检测法测定硫酸庆大霉素注射剂中有关物质

目的建立硫酸庆大霉素注射剂中有关物质的高效液相色谱-蒸发光散射检测（HPLC—ELSD）方法。方法色谱柱采用耐酸Apollo C18柱（250mm×4．6mm,5μm）,以0．2mol／L三氟醋酸溶液-甲醇（94：6）为流动相,蒸发光检测器的漂移管温度为110℃,载气流量为2．0L／min。结果硫酸庆大霉素与有关物质分离完全,可用外标法测定硫酸小诺霉素和硫酸西索米星的含量。结论所用方法准确、灵敏度高,可有效地控制药品质量。     

三油酸甘油酯的ELSD非水反相HPLC测定

运用蒸发光散射检测器(ELSD)，建立了非水反相高效液相色谱测定三油酸甘油酯(1)含量的方法。采用C18色谱柱，流动相为乙腈-异丙醇-三氟乙酸(60：40：0．05)，l中的甘油、油酸、亚油酸和另外8种有关物质可完全分离。灵敏度、精密度和回收率均好，1在0．75～2．25mg／ml浓度范围时，线性关系良好(r=0．9992)。     

硫酸卡那霉素注射液中有关物质测定方法研究

目的采用高效液相色谱-蒸发光散射检测器(HPLC-ELSD)法测定硫酸卡那霉素注射液中有关物质。方法采用ZorbaxSB-C18柱(250 mm×4.6 mm,5μm),以0.2 mol/L三氟醋酸溶液-甲醇(95∶5)为流动相,流速为1.0 mL/min,柱温为室温,用蒸发光散射检测器检测(漂移管温度为80℃,载气压力为1.0 bar)。结果以对照溶液质量浓度的对数值与相应峰面积的对数值计算回归方程,其相关系数(r)均大于0.999,二者线性关系良好。结论高效液相色谱-蒸发光散射检测器法简便、准确、专属、灵敏。     

HPLC-ELSD法测定龙牡壮骨颗粒中黄芪甲苷的含量

目的:研究龙牡壮骨颗粒中黄芪甲苷的含量测定方法.方法:高效液相色谱-蒸发光散射检测法.色谱柱为Diamonsil C18,4.6mm×250mm,5μm;流动相为甲醇-水(75:25);流速为1.0mL·min-1;柱温为30℃;检测器为Varian 380 - LC型蒸发光散射检测器.结果:该方法能很好分离被测组分与...     

HPLC-ELSD法测定复方氨基葡萄糖片中硫酸软骨素的含量

目的建立以蒸发光散射为检测器(ELSD)测定复方氨基葡萄糖片中硫酸软骨素的高效液相色谱分析方法。方法采用高效液相色谱法,以乙腈-水-三乙胺溶液(10∶90∶0.1)为流动相,ODS色谱柱为色谱柱,蒸发光散射检测器检测。结果硫酸软骨素在1.5~21μg范围与峰面积呈良好线性关系;该方法3个不同浓度的平均回收率分别为99.33%,98.29%,98.95%,重复性实验的RSD为0.15%。结论本方法准确、快速、重复性好。     

薄层扫描法测定熊胆引流物中胆汁酸含量

熊胆向以贵重药材闻名,被称之为稀有药品,为开发熊胆资源,解决熊胆奇缺问题,我校解剖教研室已成功地完成了人工引流熊胆汁技术,可随时进行人工引流获取熊胆汁。为了确定胆汁的质量指标,了解其主要成分,我们进行了引流胆汁与天然熊胆的分析。文献报道,熊胆中主要含熊去氧胆酸(ursodesoxycholic acid,UDCA)、鹅去氧胆酸(cheno desoxycholic acid,CDCA)、胆酸(cholic acid,CA)、去氧胆酸(deoxycholic,acid DCA)等。     

天然牛黄与培育牛黄的扫描电镜观察

天然牛黄(natural ox gallstone)为牛的胆结石,由于产量极少,供求困难,国内于1956年参照天然牛黄的主要成分制成人工牛黄(artificial ox gallstone),作为天然牛黄的代用品。从1974年以来,很多省区如吉林、广东、内蒙古等都先后进行了人工培育牛黄的试验,并试验成功培育牛黄(cultured ox gallstone)。其方法是用手术在牛胆囊内植入异物为核,促使胆汁成分的沉积与结石的形成,经过一段时间后,将异物取出,上面的沉积物即为培育牛黄。本文目的是探讨天然牛黄与培育牛黄的结构特征。     

熊胆粉、猪胆粉、牛胆粉及鸡胆粉中总胆酸的含量测定及其抑菌作用

目的:建立用紫外分光光度计测定熊胆、猪胆粉、牛胆粉、鸡胆粉中总胆酸含量的方法并评价抑菌效果。方法:分别以胆酸和熊去氧胆酸为对照品,采用加入硫酸-水(50∶50),在75℃水浴加热18 min反应显色,于388 nm波长处测定熊胆粉等动物胆粉中总胆酸的含量;同时以金黄色葡萄球菌和大肠杆菌为实验菌种,在650 nm波长处测定OD值以考察体外抑菌效果。结果:胆酸在5.7～34.3μg·mL-1范围内有良好的线性关系,线性方程为Y=41.573 X-0.166 1,r=0.999 5;熊去氧胆酸在4.7～23.5μg.mL-1范围内有良好的线性关系,线性方程为Y=24.957 X-0.067 9,r=0.999 6;胆酸及熊去氧胆酸在熊胆粉、牛胆粉、猪胆粉、鸡胆粉中的平均回收率及RSD值分别为:98.9%,100.5%,1.59%,1.07%;97.7%,98.8%,1.08%,1.12%;104.1%,99.4%,2.00%,1.67%;102.9%,103.6%,1.22%,1.78%。熊胆粉等4种动物胆粉对金黄色葡萄球菌和大肠杆菌均有明显的抑菌作用,但差异无显著性。结论:本法准确,简便,重复性好,可用于熊胆等4种动物胆粉中总胆酸的含量测定,熊胆等4种动物胆粉均可抑制金黄色葡萄球菌和大肠杆菌的生长。     

Free fatty acids in gallstones in mice fed a diet containing cholic acid

In mice, combined addition of 1% cholesterol and 0.5% cholic acid to a diet induced cholesterol gallstones within 40 days as a result of the supersaturation of cholesterol in the bile, as has been reported. The major component of the gallstone was cholesterol, which was measured by HPLC. In this study, however, single addition of 1% cholic acid to a diet, which did not decrease cholesterol solubilizing capacity in bile, contributed to gallstone formation in mice within 50 days. The gallstones thus formed contained a large amount of palmitic acid. In the hepatic bile of this animal, palmitic acid was also detected; however, no solid material was observed by light and polarized-light microscopes. Free fatty acids such as palmitic acid seem to be dissolved in a complex micelle composed of bile acids and lecithin. This probably causes gallstone formation by reducing cholesterol solubilizing capacity in bile.     

鸡胆汁与蛇胆汁组分的对比研究

鸡胆汁与蛇胆汁在主要成分组成上几近相同,均含有胆酸、鹅去氧胆酸、牛磺酸、甘氨酸,但含量相差较大.鸡胆汁以鹅去氧胆酸(CDCA)为主,蛇胆汁以胆酸(CA)为主;牛磺酸(Tau)蛇胆汁醇提物含量高于鸡胆汁醇提物;甘氨酸(GLY)鸡胆汁醇提物含量高于蛇胆汁醇提物.     

清开灵软胶囊中胆酸和猪去氧胆酸的含量测定

目的建立清开灵软胶囊中胆酸和猪去氧胆酸的高效液相色谱-蒸发光散射(HPLC-ELSD)含量测定方法。方法采用ShiseidoCapcell MGⅡC18色谱柱(150 mm×4.6 mm,5μm),以甲醇-乙腈-0.5%冰醋酸溶液(49∶20∶31)为流动相,流速为1.0 mL/min,柱温为25℃,蒸发光散射检测器,漂移管温度为108℃,载气流速为2.8 L/min。结果胆酸和猪去氧胆酸的进样量分别在2.338～18.704μg(r=0.999 4)和2.018～16.141μg(r=0.999 5)范围内与各自的峰面积积分值呈良好的对数线性关系,平均回收率分别为98.51%和98.01%,RSD分别为0.74%和0.72%(n=9)。结论所用方法简便、准确、分离效果好,适用于该制剂的质量控制。     

HPLC法测定胆酸和猪去氧胆酸的含量

目的:建立胆酸和猪去氧胆酸的含量测定方法.方法:采用HPLC-UV法,色谱柱为Diamonsil-C18(4.6 mm×150mm,5 μm),流动相为乙腈-水-磷酸(35:65:0.1),检测波长为192 nm,柱温25℃,流速1.5 mL·min-1.结果:胆酸、猪去氧胆酸分别在3.154～31.540μg和1.927～19.266μg线性关系良好,相关系数分别为r＝0.999 5和r＝0.999 2,平均加样回收率分别为98.98%(RSD为0.42%)和98.29%(RSD为0.61%).结论:方法准确可靠、重复性好,可用于胆酸和猪去氧胆酸的质量控制.     

Hepatic extraction of bile acids in rats

The hepatic extraction ratio (E_h) of five common bile acids was determined by comparison of the area under the plasma concentration time curve (AUC) after administration into the femoral and portal veins of rats. Taurocholic acid (TCA), glycocholic acid (GCA), cholic acid (CA), deoxycholic acid (DCA) and chenodeoxycholic acid (CDCA) were studied. Using equimolar doses of the bile acids (9.3 μmoles), the effects of both conjugation and the number and position of hydroxyl groups on E_h were compared. TCA had the highest E_h (about 80 per cent) followed in order by GCA (65 per cent), CA (55 per cent) and CDCA (55 per cent), with DCA exhibiting the lowest E_h (40 per cent). This suggests that conjugation has a more important effect on hepatic extraction of bile acids than the number of hydroxyl groups.     

A practical guide to the nonsurgical treatment of gallstones.

Until recently, cholecystectomy was the only treatment available for symptomatic gallstone disease. During the past 20 years, better understanding of the pathogenesis of cholesterol gallstone disease has led to alternative nonsurgical methods for treating gallstones in selected groups of patients. Use of 2 naturally occurring bile acids, chenodeoxycholic acid (CDCA) and ursodeoxycholic acid (UDCA), was reported in 1972 and 1975, respectively, for successful dissolution of cholesterol gallstones in humans. Both these bile acids act by reducing cholesterol secretion in bile, thus enabling it to solubilise more cholesterol from the stone surface. Micellar solubilisation is involved, together with liquid crystal formation in the case of UDCA. Having been extensively studied in clinical trials to assess efficacy and safety, both these compounds are now available for general use. The efficacy of CDCA can be enhanced by single bedtime dose administration and by taking a low cholesterol diet. Bedtime administration also enhances the effect of a suboptimal dose of UDCA. CDCA induces dose-related diarrhoea and hypertransaminaemia, and UDCA can induce calcification of gallstones, thus rendering them resistant to medical dissolution. A combination of the 2 bile acids at half the recommended dose for each has become an accepted practice for reducing adverse effects, and this may also enhance efficacy. One of the main problems of bile acid therapy is that dissolution of gallstones is a very slow process. Use of extracorporeal shockwave lithotripsy (ESWL) to break the stones into smaller fragments, with concurrent use of bile acids, has been shown to speed dissolution rate and to achieve complete gallstone dissolution in 78% of selected cases within 12 months.(ABSTRACT TRUNCATED AT 250 WORDS)     

HPLC-ELSD法同时测定护肝片中猪去氧胆酸和鹅去氧胆酸的含量

目的：建立高效液相-蒸发光散射检测（ HPLC-ELSD）法同时测定护肝片中猪去氧胆酸和鹅去氧胆酸含量的方法。方法采用Agilent Zorbax SB-C18（4.6 mm×250 mm,5μm）色谱柱,流动相为甲醇-0.2%冰醋酸溶液（80：20）,流速为1.0 mL·min-1,色谱柱温为30℃;蒸发光检测器载气为氮气,流速为2.0 L·min-1,漂移管温度为60℃。结果猪去氧胆酸在0.521~10.42μg范围内呈现良好的线性关系（ r＝0.9989）,平均加样回收率为97.41%, RSD为1.30%（n＝6）;鹅去氧胆酸在0.266~5.32μg范围内呈现良好的线性关系（r＝0.9994）,平均加样回收率为96.09%,RSD为2.11%（ n＝6）。结论该方法准确、简便、灵敏度高,可用于护肝片中猪胆粉的质量控制。