红花注射剂质量控制方法的研究

【作者】 周迎春；

【导师】 赵怀清；

【作者基本信息】 沈阳药科大学 ， 药物分析学， 2003， 硕士

【摘要】 本研究共收集了22个不同产地的红花样品，经过形态学鉴定，均为正品。本研究从红花中提取制备了羟基红花黄素A对照品，通过紫外光谱、红外光谱、质谱、核磁共振氢谱及核磁共振碳谱对其结构进行了确证，并通过HPLC归一化法测得羟基红花黄素A对照品的纯度为98.4％。应用HPLC法对不同来源的红花样品中的水溶性黄酮类化合物进行了分析：采用Kromasil KR100-5C₁₈色谱柱（250mm×4.6mm，5μm），以乙腈-0.01mol·L^-1磷酸二氢铵溶液为流动相梯度洗脱，检测波长为332nm，流速1.0 mL·min^-1。以羟基红花黄素A为参照物，建立了红花药材的HPLC指纹图谱。采用“指纹图谱相似度计算软件”分析，不同来源的红花相似度大于0.80。 本文考察了红花中红花黄素的提取分离方法。采用水为提取溶剂，并利用大孔吸附树脂对提取液进行分离、纯化。采用正交试验设计及单因素实验方法，以羟基红花黄素A的含量为指标，优化了提取工艺。该方法简便易用，成本低，适合工业化生产。 本文对提取工艺质量控制方法进行了研究。采用反相高效液相色谱法对红花黄素中的羟基红花黄素A进行了含量测定。结果表明，羟基红花黄素A在10.1～505.0μg·mL^-1范围内呈良好线性关系，相关系数r=0.9999，平均回收率为98.2％，RSD=1.3％（n=9）。本方法简单准确，灵敏度高。为提取工艺的质量控制提供了定量分析的依据。 本文在红花药材指纹图谱的基础上，采用HPLC法对实验室制备的10批红花黄素中间体和10批红花注射剂进行指纹图谱分析。采用“指沈阳药科大学硕士学位论文 摘要纹图谱相似度计算软件”分析，不同批次的的红花黄素和注射剂各自的相似度均大于0．90。为有效控制红花注射剂和中间体的质量，完善其评价标准提供依据。更多还原

【Abstract】 In this paper, 22 samples of Carthamus tinctorius were collected from different areas. It was identified that all of them were Carthamus tinctorius. First, the standard substance of hydroxysafflor yellow A was isolated from Carthamus tinctorius and the structure was elucidated by UV, IR, MS, 1H-NMR and 13C-NMR. The content of hydroxysafflor yellow A was 98.4% by HPLC. HPLC with UV detector was used to analyze the flavone in the samples of Carthamus tinctorius and hydroxysafflor yellow A was used as internal standard compound: Chromatography was performed on a Kromasil KR100-5 C18 column (250 mm×4.6 mm, 5 μm) using acetonitrile-0.01 mol .L-1 NH4H2PO4 solution as the mobile phase (gradient elution) and detected at 332 nm. The flow rate was 1.0 mL . min-1. Based on this study, HPLC fingerprint analysis method for Carthamus tinctorius was developed. Analyzing by Computer Aided Similarity Evaluation system, the similarity of Carthamus tinctorius from different areas was more than 0.80.Extraction and isolation methods of safflor yellow in Carthamus tinctorius were studied in this paper. Safflor yellow was extracted from Carthamus tinctorius by using water and isolated by using macroporous resin. By using the content of hydroxysafflor yellow A as quality control criteria, extraction and isolation process of safflor yellow in Carthamus tinctorius was optimized with the aid of orthogonal design and mono-factor trial. It was demonstrated that this method was convenient, economical and suitable for manufacture in industry.Quality control of extraction and isolation technics was studied in this paper. A RP-HPLC method was developed to determinate the content ofhydroxysafflor yellow A in safflor yellow. As a result, a good linearity was obtained from 10.1-505.0μg . mL-1 with r = 0.9999 for hydroxysafflor yellow A. The average recovery was 98.2%, RSD = 1.3% (n = 9). The method was proved to be simple, precise, sensitive.Based on the study of fingerprints of Carthamus tinctorius. HPLC method was used to analyze 10 batchs safflor yellow and safflower injection respectively. The fingerprints of safflor yellow and safflower injection were set up. Analyzing by Computer Aided Similarity Evaluation system, the similarity of safflor yellow and safflower injection was more than 0.90 respectively. The studies are useful for the quality control of safflor yellow and safflower injection.更多还原