Determination of Low Contents of Fenpiverine Bromide by Extraction Spectrophotometry

An ion-pair extraction spectrophotometry method was developed for the determination of fenpiverine bromide in tablets. To determine this substance it was necessary to find experimental conditions that would allow eliminating the influence of other components of the tablets. Attention was paid to the fact that a suitable pH of water phase was necessary to achieve high selectivity.Received December 11, 2002; accepted April 24, 2003 Published online July 28, 2003     

近红外光谱-径向基神经网络在异烟肼片无损定量分析中的应用

应用异烟肼片粉末的近红外漫反射光谱数据分别结合偏最小二乘法(PLS)和径向基神经网络(RBFNN)建立定量分析模型,并用所建模型对预测集样品进行了预测,结果表明:应用RBFNN所建立的定量分析模型优于PLS模型,相关系数(r)值由0.99593提高到0.99734,交互验证均方根误差(RMSECV)值由0.00523下降到0.00423,预测均方根误差(RMSEP)值由0.00614下降到0.00501。     

毛细管电泳法快速测定复方地芬诺酯片中的地芬诺酯和阿托品

建立了毛细管电泳高频电导法同时测定地芬诺酯和阿托品的方法。探讨了缓冲溶液、有机溶剂添加剂、分离电压和进样条件以及毛细管内径和长度等因素对分离检测的影响。在电泳介质为10.0mmol/L乳酸-15.0?H5OH、分离电压20.0kV的优化条件下,6min内即可实现地芬诺酯和阿托品的同时分离检测,线性范围分别为5.00~500和2.00~320mg/L;检出限分别为3.0和1.0mg/L。     

计算机辅助一清片径向展开薄层色谱定性与定量方法初探

径向薄层色谱法（RTLC）是一种将样品呈圆形或环状点样,然后将展开剂从中心向外沿径向输送的薄层色谱方法。在一定的展开距离内,RTLC是一种分离快速、扩散小、不拖尾的高效分离和半制备方法。目前关于RTLC分离的报道较多,但对RTLC定性和定量的报道较少。该文采用自编程方式结合图像处理软件,实现RTLC图像数字化处理,形成RTLC数字化图谱,并对RTLC进行定性与定量方法学验证,建立了一清片RTLC定性与定量方法。辅助计算机技术,对一清片径向展开薄层色谱定性与定量方法进行初探。结果表明,该方法用于RTLC定性的可靠度较好,但用于RTLC的定量,仍有不足之处,这可能与实验环境条件等有关。通过搭载更好的分离和数据采集设备,RTLC会有适合的用武之地。计算机图像处理和自编程方法的结合给了RTLC和其他一些分析相关的技术广阔的发展前景。相信未来在计算机技术的辅助下,薄层色谱技术会迈上一个新的台阶。     

近红外光谱法分析格列齐特片

应用化学计量法处理光谱数据,用偏最小二乘法建立格列齐特片的近红外分析模型。通过光谱预处理和模型的逐步优化最终确定定量分析模型的相关系数为0.991,交叉验证均方差(RMSECV)为0.641,预测均方根误差(RMSEP)为0.980,主因子数为4。选取15个验证样品对模型进行检验,检测结果相对误差在-2.04%～3.52%之间。     

离子色谱法测定复方卡托普利片中卡托普利和氢氯噻嗪的含量

建立离子色谱法测定复方卡托普利片中卡托普利和氢氯噻嗪含量的方法。在色谱柱为IonPacSCS1(4mm×250mm),保护柱为IonPacSCG1(4mm×50mm),淋洗液为甲烷磺酸(4mmol/L)+乙腈(26%),流速1.0mL/min,柱温35℃,进样量7μL,紫外检测波长215nm的条件下,测定结果表明,卡托普利和氢氯噻嗪在0.5～25μg/mL范围内线性关系良好,相关系数r分别为0.9997、0.9999,回收率分别为98.11%、94.24%。方法操作简单,灵敏度高、准确、重现性好,可用于复方卡托普利片的质量控制。     

Conductimetric,Potentiometric and Visual Titrimetric Methods for Analysis of Nadolol

Abstract

Nadolol, a beta-blocking agent, has been assayed in pure form and in pharmaceutical formulation by acidimetric titrations using visual, potentiometric and conductimetric methods for detecting the end point in aqueous as well as in non-aqueous media. The method of assay involves the determination of the amount of nadolol in a given weight of sample. Six samples were run for each method and the percentages of recovery of nadolol from its tablets were calculated. For aqueous titrations, the average percentages of recovery for the visual, potentiometric and conductimetric methods are 100.6 ± 1.0, 99.3 ± 1.9 and 100.1 ± 2.0 respectively. For the non-aqueous titrations, the average percentages of recovery are 98.6 ± 0.8, 99.5 ± 0.5 and 98.4 ± 1.3 for the visual, potentiometric and conductimetric methods respectively.     

基于线性方程组数学分离模型建立光纤传感过程检测复方缬沙坦氢氯噻嗪片溶出度

基于线性方程组数学分离模型建立在线过程检测复方缬沙坦氢氯噻嗪片溶出度方法。分别扫描缬沙坦和氢氯噻嗪的紫外吸收光谱,两组分在最大吸收波长处完全重叠。根据朗伯比尔定律吸光度加和性原理,分别测定两组分在最大吸收波长处的吸光系数,建立线性方程组数学分离模型,采用光纤传感过程分析技术(FODT)检测缬沙坦氢氯噻嗪片的溶出度,并与HPLC法相比较。在规定的溶出介质中,两种成分同时实时测定,并且FODT累积溶出度与HPLC法相比较结果无显著性差异(p>0.05)。不同批次药物的溶出行为一致,说明制剂工艺稳定,均匀度好。溶出曲线显示缬沙坦溶出快于并高于氢氯噻嗪,且30 min时两组分的溶出度均大于80%符合美国药典规定。结果表明,应用线性方程组数学分离模型结合FODT法可实现复方缬沙坦氢氯噻嗪片中双组分溶出度的同时检测,并可提供双组分的溶出过程曲线和全部溶出数据,直观反映各组分在各溶出时段的快慢,为此药建立标准提供依据。与HPLC法单点数据相比优势明显,更有利于药品评价和抽验质量分析。     

Non‐invasive probing of pharmaceutical capsules using transmission Raman spectroscopy

We demonstrate how transmission Raman geometry can be effectively used for non‐invasive probing of the content of pharmaceutical capsules. This approach is particularly beneficial in situations where the conventional Raman backscattering method is hampered or fails because of excessive surface Raman or fluorescence signals emanating from the capsule shell material, which pollute the much weaker subsurface Raman signals with undesired noise. It is demonstrated that such interfering signals can be effectively suppressed by the transmission geometry. The ability to avoid surface fluorescence and Raman signals in conjunction with the superior, bulk‐probing properties of the transmission Raman geometry provides an analytical technique ideally suited for fast on‐line process control monitoring applications in pharmaceutical industry where rapid, chemically specific bulk analysis is required. Copyright © 2007 John Wiley & Sons, Ltd.     

基于拉曼光谱法的降糖类药物的判别方法比较

采用了四种聚类方法对降糖类药物拉曼光谱进行了快速、无损判别。采集九种降糖类药品共48个样品的拉曼光谱,经截波、基线校正、平滑、矢量归一化等预处理后,分别采用K-均值、系统聚类法、自组织图(SOM)及PCA-SOM四种不同聚类方法做聚类判别。结果表明,自组织图与K-均值、系统聚类法相比,聚类结果较好,并且SOM结合PCA后的PCA-SOM结果最优。为降糖类药品的快速判别从聚类的角度提供了一种新的方法。