RP-HPLC测定黄连上清片中盐酸小檗碱含量

用反相高效液相色谱法测定中药复方制剂黄连上清片中有效成分盐酸小檗碱含量。采用Agilent 1100 ODS色谱柱(4.6mm×150mm,5μm),乙腈-0.05mol/L磷酸二氢钠溶液(用磷酸调pH值至3)(30∶70,V/V)为流动相,检测波长为345nm,流速1.0mL/min,柱温25℃。盐酸小檗碱在0.16—4.0μg/mL范围内与峰面积呈良好的线性,r=0.9999,平均加样回收率为98.96%(n=6),RSD=1.09%。该法快速简便,灵敏度和稳定性高,可有效控制黄连上清片的内在质量。     

反相高效液相色谱法测定清开灵分散片中栀子苷含量

对中药复方制剂清开灵分散片中有效成分栀子苷进行含量测定。采用反相高效液相色谱法,Agilent1100ZORBAXEclipseXDB-C18色谱柱(4.6mm×150mm,5μm),乙腈-水(15∶85,V/V)为流动相,检测波长为238nm,流速1.0mL/min,柱温25℃。栀子苷在0.0593—1.4825μg.mL-1范围内与峰面积呈良好的线性关系,r=0.9999,平均加样回收率为98.93%(n=6),RSD=1.21%。该方法快速简便、灵敏度和稳定性高,可有效控制清开灵分散片的内在质量。     

紫外光纤化学传感原位过程监测青霉素V钾片溶出度

考察了光纤传感溶出度仪监测青霉素V钾片的溶出过程.结果表明方法的日内、日间精密度,回收率符合分析测试的要求,并与中国药典的方法比较,TD、T50及累积溶出率均无显著性差异(P＞0.05).光纤化学传感检测提高了测定的精密度和准确度,获得的数据信息完整,反映了药物在体外溶出的过程,替代了繁琐的传统测试方法.     

Analysis of levofloxacin in pharmaceutical preparations by high performance thin layer chromatography

A new simple, precise, rapid, and selective high‐performance thin layer chromatography (HPTLC) method has been developed for the analysis of levofloxacin in pharmaceutical formulations. The method uses lamotrigine as an internal standard. The stationary phase was silica gel 60F₂₅₄ prewashed with methanol; water‐methanol‐n‐butanol‐ammonia solution 5 + 5 + 5 + 0.4 (v/v) was used as mobile phase. Detection and quantification were performed densitometrically at λ = 298 nm. The linear range of the analysis was 0.8–3.0 μg and the percentage recovery was 99.90%.     

High Pressure Liquid Chromatographic Analysis and Dissolution of Famotidine in Tablet Formulation

Abstract

A reversed phase high pressure liquid chromatographic method was developed for the quantitation of famotidine in tablet formulation using a mobile phase consisting of 0.1M phosphate buffer (84%), acetonitrile (11%) and methanol (5%) at a pH of 6.5. The detection wavelength was set at 285 nm. The method is precise and adaptable for quality control purposes. The use of the analytical method hi studying tablet dissolution is described.     

Robust calibrations on reduced sample sets for API content prediction in tablets: Definition of a cost-effective NIR model development strategy

Owing to spectral variations from other sources than the component of interest, large investments in the NIR model development may be required to obtain satisfactory and robust prediction performance. To make the NIR model development for routine active pharmaceutical ingredient (API) prediction in tablets more cost-effective, alternative modelling strategies were proposed. They used a massive amount of prior spectral information on intra- and inter-batch variation and the pure component spectra to define a clutter, i.e., the detrimental spectral information. This was subsequently used for artificial data augmentation and/or orthogonal projections. The model performance improved statistically significantly, with a 34–40% reduction in RMSEP while needing fewer model latent variables, by applying the following procedure before PLS regression: (1) augmentation of the calibration spectra with the spectral shapes from the clutter, and (2) net analyte pre-processing (NAP). The improved prediction performance was not compromised when reducing the variability in the calibration set, making exhaustive calibration unnecessary. Strong water content variations in the tablets caused frequency shifts of the API absorption signals that could not be included in the clutter. Updating the model for this kind of variation demonstrated that the completeness of the clutter is critical for the performance of these models and that the model will only be more robust for spectral variation that is not co-linear with the one from the property of interest.     

Analysis and stability of polymorphs in tablets: The case of Risperidone

Identification of the crystal phase of an active pharmaceutical ingredient (API) in a pharmaceutical tablet is of outmost importance since different polymorphs exhibit different physicochemical properties. Furthermore, some of the crystal phases are protected by patents. Identification of Risperidone polymorph A in film coated commercial tablets was attempted using IR spectroscopy, Raman spectroscopy and X-ray powder diffraction (XRPD). The stability of this polymorph through time and during the manufacturing process was also examined. The inability of IR and Raman techniques to identify the presence of polymorph A in the tablets, despite their lower detection limits for Risperidone, left the XRPD as the only technique that could be used for identifying the presence of Risperidone A against the other crystal phases in the presence of the excipients. Polymorph A was proved to be stable during the manufacturing process and after a storage period of 2 years.     

3种不同提取方法测定百癣夏塔热片中的总黄酮

采用索氏提取、超声提取、微波萃取对百癣夏塔热片中总黄酮进行提取.3种方法均采用20倍(mL/g)甲醇;其中索氏提取时间为6h;超声提取时间为1h;微波萃取辐射时间:10min;温度:100C.以芦丁为标准品,用分光光度法测定,波长为510nm,芦丁浓度与吸光度呈良好的线性关系(r=0.9999).微波萃取、索氏提取和超...     

HPLC测定山楂精降脂片中的齐墩果酸和熊果酸

采用十八烷基硅烷键合硅胶为固定相,以乙腈-甲醇-0.5%醋酸铵溶液（67∶12∶21）为流动相,检测波长为210nm。齐墩果酸在0.0195—0.78μg范围内线性关系良好（r=0.9997）,回收率为98.76%（RSD为0.76%）;熊果酸在0.081—3.24μg范围内线性关系良好（r=0.9999）,回收率为99.04%（RSD为0.80%）。本方法简便、快速,结果准确,可用于山楂精降脂片的质量控制。     

光纤传感技术结合紫外光谱快速检验马来酸氯苯那敏片

建立一种光纤传感技术结合紫外-可见吸收光谱快速定性、定量分析药物的方法.将光纤探头浸入待测药物溶液中,氘灯光源发出的光通过光纤传输到探头,由探头感受经溶液吸收的光信号,并再次通过光纤反馈到检测器,最终通过计算机即时显示待测药物的光纤紫外-可见吸收光谱,并利用光谱中最大、最小吸收波长及吸光度与对比图谱比较获得定性、定量信...