摘要：苯磺贝他斯汀是一种高效的组胺H1受体拮抗剂，可有效缓解鼻塞、流涕、喷嚏等临床症状，还可用于治疗荨麻疹、皮肤炎症引起的瘙痒、神经性耳鸣等，起效快，无镇静作用,其他不良反应极小，临床药效均优于同类药物，因此具有广泛的应用前景。本课题的目的是建立一个简单、准确、精密且稳定性好的进行原料药苯磺贝他斯汀的含量测定的方法。通过对色谱柱类型、紫外检测波长、色谱柱温度、进样体积、流速、流动相的组成及比例等的筛选，确立最佳色谱分析条件，即采用Kromasil100-5-C18(250×4.6mm，5μm)色谱柱，检测波长220nm，色谱温度为35oC，流速1.0mL·min-1，洗脱方法为缓冲液-乙腈先以(75%-25%)(v/v)洗脱8min，之后梯度洗脱12min将缓冲液-乙腈比例改变为(40%-60%)(v/v)。经方法学验证，即通过系统适应性试验、精密度试验、准确度试验等一系列试验，证实该方法简单、精确、稳定性和重现性好。
关键词：苯磺贝他斯汀；高效液相色谱；最佳色谱条件；方法学验证
Study on analytical method of Bepotastine Besilate(API)
Abstract: Bepotastine Besilate is a high performance histamine H1 receptor antagonist. It can remission the symptom of rhinobyon, rhinocnesmus and sternutation, and it can also be used to dealing with urticarial, pruritus caused by dermatitis, nervous tinnitus and so on. It takes effect quickly and has few other untoward effect. The pesticide effect and clinical effect of bepotastine besilate is better than other drugs of the same kind, which lead to a broad application prospect of it. The purpose of this research is to develop a simple, accurate, precise and robust method to determine the content of bepotastine besilate (active pharmaceutical ingredient). By selecting the type of chromatographic column, chromatographic detection wavelength, chromatographic column temperature, flow rate, injection volume as well as composition and proportion of mobile phase to determine the optimum analysis condition. The chromatographic analysis was performed on Kromasil 100-5-C18 (250 × 4.6 mm，5μm) with detection wavelength in 220 nm. The column temperature is 35 oC and flow rate is 1.0 mL·min-1. The elution method is adjusting the mobile phase A ( pH = 3.0 phosphate buffered saline) and mobile phase B in a proportion of (75% - 25%) (v / v) initially, and then change the proportion of mobile phase A and mobile phase B to (40% - 60%) (v / v) in the following 12 min. The analysis method is validated by methodology validation such as system stability test, precision test, accuracy test and so on. Hence the developed method is accurate, simple, robust and reproducible.
Key Words: Bepotastine Besilate; High Performance Liquid Chromatography; optimum analysis condition; methodology validation
目录
1前言.1
1.1苯磺贝他斯汀的开发..1
1.2苯磺贝他斯汀的药用机理及效用.1
1.3苯磺贝他斯汀的合成方法.2
1.4高效液相色谱及其在药物分析中的应用.3
1.4.1高效液相色谱的特点.3
1.4.2高效液相色谱简介4
1.4.3高效液相色谱在药物分析中的应用.5
1.6本课题的研究目的和意义.7
2实验部分8
2.1材料与仪器.8
2.1.1材料与试剂8
2.1.2仪器与设备9
2.2内容与方法.9
2.2.1实验设计思路.9
2.2.2仪器操作方法.9
2.2.3溶液的配置..10
2.2.4药物的前处理11
3结果与讨论..11
3.1苯磺贝他斯汀含量测定色谱条件筛选..11
3.1.1最大吸收波长的选择11
3.1.2色谱柱的选择12
3.1.3色谱柱温度的选择..13
3.1.4进样体积的选择.15 苯磺贝他斯汀的分析方法研究:http://www.chuibin.com/huaxue/lunwen_205344.html