高效液相色谱法测定复方丹参片和滴丸中丹酚酸B和丹参酮ⅡA的含量

目的:测定复方丹参片和复方丹参滴丸中丹酚酸B和丹参酮ⅡA的含量,比较两种丹参制剂的内在质量区别.方法:采用高效液相色谱(HPLC)方法测定丹酚酸B和丹参酮ⅡA在两种制剂中的含量.结果:复方丹参片中丹酚酸B和丹参酮ⅡA的含量比复方丹参滴丸中的含量高.结论:两种丹参制剂的内在质量差别很大.     

临床常用丹参制剂活性成分比较分析

目的 分析临床常用丹参制剂,包括复方丹参片、丹参片、冠心丹参滴丸、复方丹参滴丸、丹参注射液、丹香冠心注射液和注射用丹参冻干粉等,主要活性成分组成和含量差异。方法 采用Kinetex柱(100 mm×4.6 mm,2.6 μm),以0.1%三氟乙酸水—乙腈为流动相,柱温为30℃梯度洗脱,丹酚酸类检测波长280 nm,丹参酮类为254 nm;测定丹参制剂中9种酚酸和4种丹参酮类成分的含量。结果 复方丹参片、丹参片、复方丹参滴丸和冠心丹参滴丸等口服制剂化学成分组成与丹参药材相似,酚酸类成分主要为丹酚酸B,丹参酮类主要为丹参酮Ⅱa。丹参注射液和注射用丹参冻干粉中主要酚酸类成分为丹参素,检测不到丹参酮类成分。 结论 不同组方和不同厂家丹参制剂活性成分组成和含量有明显差异。口服制剂中成分与丹参药材相似,而注射制剂中主要含丹酚酸类成分,检测不到丹参酮类成分。     

高效液相色谱法测定复方丹参片与滴丸中7种活性成分含量

目的：建立高效液相色谱( HPLC)法同时测定复方丹参片和复方丹参滴丸中7种活性成分含量的方法。方法采用Zorbax C18色谱柱,以乙腈-0.1％磷酸溶液为流动相,梯度洗脱,流速1 mL·min-1,检测波长为203,270和281 nm。结果7种成分峰面积与浓度的线性关系良好;加样回收率在95.1％~100.4％;滴丸样品中丹参酮ⅡA未能检出。结论建立了两类复方丹参制剂中同时测定丹参素、原儿茶醛、三七皂苷R1、人参皂苷Rg1、丹酚酸B、人参皂苷Rb1和丹参酮ⅡA含量的方法,精密度高,重复性好,可用于两类复方丹参制剂的质量控制;复方丹参片中丹参酮ⅡA含量明显高于滴丸。     

32批丹参饮片的质量考察

目的：考察丹参饮片的质量。方法：对32批丹参饮片中的丹参酮ⅡA和丹酚酸B作含量测定。结果：32批丹参饮片中丹参酮ⅡA含量较低,丹酚酸B含量较高,但丹酚酸B含量的高低差异较大。结论：应加强丹参饮片的内在质量管理。     

复方丹参片与滴丸中丹酚酸B和丹参酮Ⅱ_A含量的比较研究

目的:测定并比较复方丹参片与滴丸中丹酚酸B和丹参酮ⅡA的含量。方法:色谱柱为EclipseXDBC18,丹酚酸B、丹参酮ⅡA流动相分别为甲醇-0·2%磷酸溶液(40∶60)、甲醇-水(85∶15),流速为1·0ml/min,柱温为30℃,检测波长为280nm。结果:丹酚酸B和丹参酮ⅡA进样量均在0·1μg~2·0μg范围内与峰面积值呈良好线性关系(r丹酚酸B=0·9998、r丹参酮ⅡA=0·9999);复方丹参片中丹酚酸B、丹参酮ⅡA的平均回收率分别为100·7%(RSD=1·9%)、101·0%(RSD=1·5%),复方丹参滴丸中丹酚酸B、丹参酮ⅡA的平均回收率分别为98·6%(RSD=1·2%)、98·8%(RSD=1·4%)。结论:本方法准确、可靠、重现性好;复方丹参片中丹酚酸B和丹参酮ⅡA含量较高,复方丹参滴丸中则未定量检出上述2成分。     

反相高效液相色谱法同时测定抗小叶增生合剂丹酚酸B和丹参酮ⅡA的含量

抗小叶增生合剂是一种用于治疗乳腺增生症且疗效独特的医院制剂,临床疗效好[1].其处方中丹参所含有效成分可分为脂溶性的丹参酮类(丹参酮ⅡA和隐丹参酮)及水溶性的丹参酸类(丹酚酸B).按2005年版<中国药典>这2种成分,作为药材丹参的质量控制指标.本研究用反相高效液相色谱法测定该制剂中丹酚酸B和丹参酮ⅡA的含量.     

HPLC法测定不同采收期丹参中丹参酮ⅡA及丹酚酸B含量

目的测定同一产地不同采收期丹参药材中丹参酮ⅡA及丹酚酸B的含量。方法以丹参酮ⅡA和丹酚酸B为定量评价指标,高效液相色谱法进行含量测定。结果 6批次丹参药材中丹参酮ⅡA质量分数为0.23%～0.36%,平均为0.29%;10批次丹参中丹酚酸B的质量分数为3.59%～4.48%,平均为3.97%。结论相同产地不同采收期丹参药材中丹参酮ⅡA及丹酚酸B的含量存在一定差异。     

广东梅州引种丹参质量初步评价

目的研究梅州引种丹参丹参酮ⅡA与丹酚酸B含量。方法采用HPLC法,测定了梅州市引种丹参的丹参酮ⅡA和丹酚酸B含量。结果本市引种品种的丹参酮ⅡA和丹酚酸B含量均达到药典规定标准。结论本市引种的丹参植株丹参酮ⅡA和丹酚酸B含量达到药典标准,适合在本地推广种植。     

丹参制剂中丹参不同提取方法的合理性评价

目的:对含丹参中药制剂中丹参不同提取方法的合理性进行评价研究。方法:以丹参片、复方丹参片、复方丹参滴丸、冠心丹参片中丹参的提取方法为研究对象,比较采用不同提取工艺、浓缩温度和溶剂对丹参中指标成分(丹参酮ⅡA、丹酚酸B)的提取量和浓缩前后指标成分含量的影响。结果:丹参采用90%乙醇渗漉法提取,指标成分提取量最大;浓缩温度对95%醇提取液中丹参酮ⅡA稳定性影响较小,而对水提取液中丹酚酸B稳定性影响较大;不同方法提取的丹参提取液浓缩后指标成分含量均不同程度降低。结论:丹参采用不同方法提取后指标成分的含量差异较大,浓缩对指标成分的含量变化影响较大。因此,针对相同或相近功效的丹参制剂,应统一丹参的提取浓缩方法。     

替代对照品法用于丹参和复方丹参片含量测定的研究

目的:建立HPLC替代对照品法测定丹参和复方丹参片的含量。方法:选取对羟基苯甲酸甲酯作为丹参和复方丹参片含量测定对照品丹酚酸B的替代对照品,在不同的条件下测定替代对照品相对对照品的校正因子,利用校正因子和替代对照品对羟基苯甲酸甲酯进行丹参和复方丹参片中丹酚酸B的含量测定。结果:丹酚酸B和对羟基苯甲酸甲酯进样量分别在0.09～2.71μg(r=1.0000)和0.015～0.45μg(r=1.0000)内与峰面积呈良好的线性关系(n=7),测得校正因子f=5.2884,用替代对照品测定方法测得回收率为100.5%(n=9)。结论:本文首次在高效液相色谱仪上使用替代对照品测定了丹参和复方丹参片中丹酚酸B的含量,结果证明用替代对照品对于丹参和复方丹参片进行药品质量控制是可行的、实用的。     

不同厂家复方丹参片的体外溶出度比较

目的：比较3个厂家复方丹参片的溶出度,考察其质量。方法：采用浆法进行体外溶出度试验。以高效液相色谱测定丹酚酸B的含量,计算其累计溶出百分率,并以威布尔方程拟合溶出参数,用方差分析进行统计学处理。结果：3个厂家复方丹参片的溶出度差异显著（P〈0．05）。结论：不同药厂复方丹参片的质量存在差异,临床用药时应加以注意。     

复方丹参pH依赖型延迟释药微丸在家犬体内的药效动力学

目的制备复方丹参pH依赖型延迟释药微丸填充胶囊并进行家犬体内药效动力学研究。方法分别用HPMC，Eudragit L-30D-55，Eudragit L100/S100 (1∶6)包衣制备pH依赖型延迟释药微丸，测定体外释放曲线，并用血清药理学方法进行家犬体内的药效动力学研究。结果制备了复方丹参pH依赖型延迟释药微丸，体外溶出曲线呈pH依赖特征。单剂量给药后自制速释片R的药效动力学参数T_max为0.58 h，E_max为34.63%，延迟释药胶囊T1和T2的T_max分别延长至2.42和3.17 h，E_max分别降低至13.57%和14.52%，相对生物利用度分别为99.3%和133.6%。多剂量给药后自制速释片R波动度DF 7.32，延迟释药胶囊T1和T2的波动度DF 3.40和3.03。结论复方丹参pH依赖型延迟释药胶囊体外释放具有pH依赖特征，体内具有明显的延迟释药作用，多剂量达到稳态时，药效动力学波动系数低于普通片。     

Salvianolic acid B, an aqueous component of danshen (Salvia miltiorrhiza), relaxes rat coronary artery by inhibition of calcium channels

In this study, we have investigated the mechanism of action through which salvianolic acid, a constituent of the medicinal herb danshen (Salvia miltiorrhiza), causes relaxation of isolated coronary artery rings precontracted with 1 microM 5-hydroxytryptamine (5-HT). The vasorelaxant effects of salvianolic acid B were also compared with the aqueous extract of danshen. Extraction of the water-soluble fraction from danshen provided a yield of 17.5%. The amount of salvianolic acid B determined in this aqueous extract was 3.9%, and the extract was 6.3 times less potent than salvianolic acid B in relaxing 5-HT-precontracted coronary artery rings; IC(50) values were 930.3+/-133.5 microg/ml and 147.9+/-17.4 microg/ml, respectively. Removal of the endothelium did not significantly affect their vasodilator potencies; IC(50) values were 842.1+/-123.8 mictog/ml and 160.3+/-25.9 microg/ml. On the other hand, a potassium channel inhibitor tetraethylammonium (TEA, 10 mM) shifted their concentration-response curves by 1.7 and 2.9 folds. The possible involvement of Ca(2+) channels was investigated in artery rings incubated with Ca(2+)-free buffer and primed with 1 microM 5-HT or 60 mM KCl for 5 min prior to adding CaCl(2) to elicit contraction. In 5-HT-primed preparations, 2 mg/ml danshen aqueous extract and 0.72 mg/ml salvianolic acid B abolished the CaCl(2)-induced vasoconstriction, whereas, in KCl-primed preparations, 10 mg/ml danshen aqueous extract and 1.44 mg/ml salvianolic acid B produced 90% inhibition. These findings suggest the vasorelaxant effects of danshen aqueous extract and salvianolic acid B were produced by inhibition of Ca(2+) influx in the vascular smooth muscle cells. The opening of K(+) channels had a minor contribution to their effects, but endothelium-dependent mechanisms were not involved. The high vasodilator potency and the quantity of salvianolic acid B contained in danshen aqueous extract suggest it is an important vasodilator constituent in this medicinal herb.     

精制冠心片超高效液相色谱法特征图谱的研究

目的：建立精制冠心片的特征图谱。方法：采用UHPLC法。采用Dikma Endevaorsil C₁₈色谱柱（2.1 mm×100 mm,1.8 μm）,柱温30 ℃,流速0.2 mL·min^-1,流动相为乙腈-0.05%磷酸溶液,梯度洗脱,检测波长为270 nm。结果：建立了以丹酚酸B,丹参酮IIA为参照峰的精制冠心片的特征图谱,并指认了芍药苷、迷迭香酸、丹酚酸B、藁本内酯、隐丹参酮和丹参酮IIA 6个特征峰。结论：精制冠心片特征图谱的建立,可以更好地控制精制冠心片的质量。     

不同厂家复方丹参注射液质量考察

目的:考察不同厂家、不同批次复方丹参注射液的质量差异。方法:采用高效液相色谱法进行梯度洗脱得到复方丹参注射液的指纹图谱;测定不同厂家、不同批次样品中丹参素、原儿茶醛、丹酚酸B的含量,并按照《中国药典》2005年版要求检查样品中不溶性微粒、蛋白质、鞣质、树脂等物质。结果:复方丹参注射液指纹图谱特征明显;不同厂家样品中丹参素、原儿茶醛、丹酚酸B含量有显著性差异,部分产品的有关物质不符合规定。结论:不同厂家的复方丹参注射液存在质量差异,应加强和统一复方丹参注射液的质量控制标准,在工艺和技术上对不溶性微粒的控制进行研究和改进。     

2种治疗方案治疗中风后遗症的成本-效果分析

目的：评价复方丹参片与胞磷胆碱钠注射液治疗中风后遗症的经济学效果。方法：将104例中风后遗症患者,随机分为A组（复方丹参片,54例）和B组（胞磷胆碱钠注射液,50例）,观察2组的临床效果,并运用药物经济学比较其成本-效果。结果：A组治疗成本为48元,有效率为83%;B组治疗成本为1632元,有效率为80%,2组成本-效果比分别为0.58和20.4。以A组为参照的增量成本-效果比为-528。结论：与胞磷胆碱钠注射液比较,复方丹参片治疗中风后遗症疗效相当,但经济性较好。     

Contents of four active components in different commercial crude drugs and preparations of Danshen （Salvia miltiorrhiza）

AIM:To detect the contents of four active components of Salvia miltiorrhiza in various commercially available danshen crude drugs and preparations.METHODS:Commercially available danshen crude drugs from different sources,as well as danshen pills and intravenous injection preparations containing danshen alone or in combination with other herbs were collected.The composition of these danshen samples was analyzed using HPLC.Specifically,the amounts of magnesium tanshinoate B(MTB),danshensu,isotanshinone IIA,and cryptotanshinone were determined.In some of these samples,the content of MTB was further confirmed by liquid chromatography-tandem mass spectrometer (LC-MS)/MS method.RESULTS:There were great variations in the amount of the four active ingredients in the commercially available danshen crude drugs and drug preparations in this study.The amount of MTB was the highest among the four components measured in the crude drugs.However,the amounts of MTB in all danshen preparations were much lower than those in crude drugs.The 2 lipophilic components,isotanshinone IIA and cryptotanshinone,were very low or not detectable in both injection and oral preparations.CONCLUSION:MTB can be used to standardize the various forms of danshen crude drugs and drug preparations from different sources.In view of the variation in the amounts of MTB and other components,improvement in the production methods of danshen preparations is essential to ensure consistent amount of its active ingredients and reproducible pharmacological actions.