【作者】 陶春梅；

【导师】 于治国；

【作者基本信息】 沈阳药科大学 ， 药物分析学， 2006， 硕士

【摘要】 本研究采用高效液相色谱法，对注射用丹红及其两味药材进行了色谱指纹图谱的研究，并对注射剂的质量标准加以完善。建立了注射用丹红色谱指纹图谱分析方法。采用Apollo-C₁₈柱（250 mm×4.6 mm，5μm），以水（含1％冰醋酸1％四氢呋喃）-乙腈为流动相梯度洗脱，流速0.8 mL·min^-1，检测波长280nm，柱温25℃，进样量10μL。实现了对注射用丹红中12个色谱峰的分离，绘制了HPLC指纹图谱共有模式。分别以夹角余弦和相关系数为测度，对不同批注射用丹红试制品进行相似度计算。10批注射用丹红的HPLC指纹图谱相似度均在0.90以上。分别建立了注射用丹红中的两味药材的HPLC指纹图谱共有模式，实现了对丹参中12个色谱峰、红花中22个色谱峰的有效分离。分别以夹角余弦和相关系数为测度，经对不同批次的药材与共有模式的相似度计算，15批不同产地的丹参、14批不同来源的红花药材HPLC指纹图谱相似度均在0.80以上。建立了注射用丹红中丹参素、原儿茶醛、红花黄色素A和丹酚酸B含量的同时测定法。采用Apollo-C₁₈柱，以水（含1％冰醋酸）-乙腈为流动相，进行梯度洗脱，检测波长为280nm，柱温25℃。四种指标成分的线性范围分别为丹参素：1.12～11.2μg·mL^-1（r=0.9997）；原儿茶醛：0.256～2.56μg·mL^-1（r=0.9996）；红花黄色素A：3.46～34.6μg·mL^-1（r=0.9995）；丹酚酸B：36.2～362μg·mL^-1（r=0.9997）。回收率分别为丹参素99.5％（RSD=1.9％）；原儿茶醛101.0％（RSD=3.0％）；红花黄色素A 98.8％（RSD=2.1％）：丹酚酸B 100.7％（RSD=1.8％）。经对10批试制注射用丹红样品测定，丹参素、原儿茶醛、红花黄色素A和丹酚酸B含量分别为：1.35～2.17 mg·支^-1；0.230～0.430 mg·支^-1；4.11～7.62 mg·支^-1；37.9～60.5 mg·支^-1。在该色谱条件下实现了对丹参药材进行丹参素、原儿茶醛和丹酚酸B的同时测定。经方法学考察，该法适用于丹参药材的质量控制。经对15批丹参药材测定，丹参素、原儿茶醛和丹酚酸B的含量分别为：1.41～2.68 mg·g^-1；0.221～0.467 mg·g^-1；52.36～84.78 mg·g^-1。采用Apollo-C₁₈柱，以水（含0.5％冰醋酸）-乙腈为流动相，对红花药材中的红花黄色素A进行含量测定。经方法学考察，本法的线性范围为9.24～92.4μg·mL^-1（r=0.9997），平均回收率为100.3％（RSD=1.6％）。经对14批红花药材分析，红花黄色素A的含量为6.5～19.3mg·g^-1。本研究建立了注射用丹红和两味药材的综合评价质量方法，为其质量标准的建立提供了依据。更多还原

【Abstract】 Quality control of Danhong for injection and two kinds of Traditional Chinese Medicines were developed by HPLC method.A method for the HPLC fingerprints of Danhong for injection by high performance liquid chromatography with UV detection at 280 nm is established, In the HPLC fingerprints of Danhong for injection 12 peaks were separated using gradient HPLC. The column to be used was Apollo-C₁₈,4.6 mmx250 mm, 5μm and the mobile phase was acetonitrile and 1%HAc and 1%THF. Common fingerprint was obtained. The similarities of 10 batches of Danhong for injection were determined by Cosine and Correlation, respectively. The results of similarity analysis were 0.90～1.00.With the methods of HPLC two kinds of Traditional Chinese Medicines were analyzed by chromatographic fingerprints. 12 peaks in Salvia miltiorrhiza Bge., 22 peaks in carthamus tinctorius L. were separated and Common fingerprint were obtained. The similarities were determined by Cosine and Correlation, respectively. The results of similarity analysis were 0.80～1.00.A reversed-phase HPLC method was developed for determination of 4 water-soluble components, danshensu, protocatechuic aldehyde, safflor yellow A and salviamolic acid B in Danhong for injection. Apollo-C₁₈ was used as the stationary phase, and The mobile phase was composed of acetonitrile and 1% acetic acid with gradient elution and the flow rate was 1.0 mL-min’1. The detection wavelength was at 280 nm and column temperature was 25℃. The linear ranges of danshensu, protocatechuic aldehyde, safflor yellow A and salviamolic acid B were 1.12～112μg·mL^-1,0.256².56μg·mL^-1,3.46～34.6 ug·mL^-1 and 36.2～362μg·mL^-1 （r≥0.9995）, respectively. The average recoveries were 99.5%, 101.0%, 98.8% and 100.8%（RSD<3.0%, n=9）, respectively. The content of 10 batches of Danhong for injection were 1.35～2.17 mg; 0.230⁰.430 mg; 4.11～ 7.62 mg; 37.9～60.5 mg per injection. Base on this method, danshensu, protocatechuic aldehyde and salviamolic acid B were determined in 10 batches of Salvia miltiorrhiza Bge.. The content were 1.41～2.68 mg·g^-1; 0.221～0.467 mg·g^-1; 52.36～84.78 mg·g^-1.A reversed-phase HPLC method was developed for determination of safflor yellow A in carthamus tinctorius L. An Apollo-C₁₈ column（250 mm×4.6 mm, 5μm） was used, with the mobile phase of acetonitrile-water-acefic acid （10: 90: 0.5, v/v/v） and flow rate of 1.0 mL·min^-1, The eluate was monitored with UV absorption at 402 nm. The linear ranges of safflor yellow A was 9.24～92.4μg·mL^-1（r=0.9997）, and the average recovery was 100.3%（RSD=1.6%）. The content of 14 batches of carthamus tinctorius L. were 6.5～19.3 mg·g^-1.Conclusively, the quality assessment methods of Salvia miltiorrhiza Bge., carthamus tinctorius L. and Danhong for injection were developed, which provided a basis for the establishment of quality control of them.更多还原