不同提取工艺对复方中东莨菪碱含量的影响

目的 探讨不同提取工艺对复方中东莨菪碱含量的影响.方法 根据喘平复方中主要成分的性质,设计了6种提取工艺.采用高效液相色谱法,以东莨菪碱的含量为指标,考察6种工艺对复方中东莨菪碱的提取及转移率.结果 0.05％盐酸的提取及转移率都较好.结论 0.05％盐酸提取工艺简单高效,适合工业化生产.高效液相色谱法测定东莨菪碱专属性好、准确、稳定可靠.     

未来的药物治疗学;药物、剂型和给药系统的发展趋向

在过去二、三年里,许多有意义的具有独特性能的新剂型和给药系统已经投放市场,标志着在药物治疗上比过去二、三十年有更为重要的进展。由皮肤途径给药获得的突破性进展已收到效果,过去的一年中已销售了三种不同的硝酸甘油给药装置以及治疗晕动病的经皮给药的东莨菪碱制剂。不久的将来,     

市售羟基喜树碱制剂的含量考查

目的:考查几种市售羟基喜树碱制剂的含量.方法:用高效液相紫外检测法对来源于9个厂家14个批次的羟基喜树碱制剂进行含量比较.结果:羟基喜树碱和内标保留时间分别为4.8min和6.5min,标准曲线在0.5～10μg·mL-1范围内线性关系良好.各厂家制剂含量在73%～98%之间.结论:该法适用范围广;相同剂型不同厂家的产品含量有差异.     

高效液相色谱法测定茶叶中儿茶素含量

［摘要］目的建立茶叶中3种儿茶素检测方法,比较目前市场不同品种茶叶中儿茶素含量差异性。方法采用改进的高效液相色谱（HPLC）法测定了不同茶叶中3种儿茶素的含量,对5个不同品种茶叶进行了儿茶素含量差异性检查。色谱柱为Hypersil BDS C18（250 mm×4.6 mm,5 μm）柱;流动相为乙腈：0.1%柠檬酸溶液＝10：90;柱温30 ℃,波长280 nm。结果改进的HPLC方法测定3种儿茶素在2～400 mg•L 1范围内线性关系良好（r＞0.999）,平均回收率＞99.0%,精密度＜2.0%。结论不同品种茶叶中儿茶素含量变化差异性较显著。建议进一步研究和完善茶叶的采摘、加工及贮存等流程,并制定出科学、合理的质量标准。     

益肾健骨胶囊的质量标准研究

［摘要］目的建立益肾健骨胶囊的质量标准。方法在原剂型标准基础上对大黄素、甘草次酸、淫羊藿苷、人参皂苷Rg1鉴别方法进行改进,同时增加了丹参的薄层色谱鉴别;取消原剂型齐墩果酸含量测定方法,增加了淫羊藿苷的测定。结果薄层图谱斑点清晰,阴性无干扰;淫羊藿苷进样量在0.104 1～1.561 5 μg范围内线性关系良好,r＝0.999 9,平均加样回收率为98.76%,RSD为1.63%（n＝6）。结论该方法操作简便,结果可靠,重复性好,可用于该药的质量控制.     

阿仑膦酸钠药物的分析

目的对国内外阿仑膦酸钠药物的各种分析方法及其原理、优缺点进行总结概括,并对阿仑膦酸钠新剂型含量测定进行探讨。方法以国内外有代表性的论文为依据,进行分析、整理和归纳。结果现有的分析方法解决了阿仑膦酸钠难以检测的难题,人们根据阿仑膦酸钠分子结构,已完成了不同阿仑膦酸钠检测方法的建立。不同的检测方法根据不同的检测机制,具有不同的检测灵敏度,在使用过程中根据具体需要适当的选择。结论阿仑膦酸钠不同分析方法的建立为进一步深入研究阿仑膦酸钠奠定了基础,也为阿仑膦酸钠衍生物、新剂型的研究提供了依据。     

注射用丁溴东莨菪碱的制备及稳定性考察

目的:探讨注射用丁溴东莨菪碱的处方组成、制备工艺、测定方法及稳定性。方法:以甘露醇为填充剂,制备注射用丁溴东莨菪碱;采用高效液相色谱法测定其含量和有关物质。结果:最佳处方为主药20mg,甘露醇20mg;高温、强光对本品均有不利影响;密闭,在凉暗干燥处保存2年无明显变化。结论:经中试放大制备的注射用丁溴东莨菪碱性质稳定、质量可控。     

硝酸甘油制剂的进展

目前,国内硝酸甘油的制剂仅有舌下片、舌下膜剂和其乙醇溶液剂,国外本品剂型较多。由于药物剂型不同,给药方法则不同,药代动力学也不一样,在临床上的疗效就有差异;又因本品具有挥发性及药片间的互相迁移和包装材料的吸附,常使药物含量下降,导致疗效降低。对此,国内外对     

注射用丁溴东莨菪碱在木糖醇和果糖注射液中的配伍稳定性考察

目的考察注射用丁溴东莨菪碱在木糖醇注射液和果糖注射液中的配伍稳定性。方法将临床常规剂量注射用丁溴东莨菪碱分别加入木糖醇注射液和果糖注射液中,室温下放置6 h,观察外观,测定pH值及不溶性微粒数,并采用高效液相色谱法测定配伍后不同时间点溶液中丁溴东莨菪碱含量。结果 6 h内2种配伍液的外观、pH值及丁溴东莨菪碱含量无明显改变,不溶微粒数符合中国药典规定。结论注射用丁溴东莨菪碱可以与木糖醇注射液和果糖注射液配伍使用。     

氢溴酸东茛菪碱的含量和降解产物的测定

目的:采用离子对色谱法测定氢溴酸东莨菪碱注射液的含量和降解产物.方法:以ODS柱为固定相,0.004%磷酸溶液(pH3.0)-乙腈(50:50)配制的0.008 mol·L-1十二烷基硫酸钠溶液为流动相,流速1.0 mL·min-1,用DAD检测器于波长210 m处测定.结果:氢溴酸东莨菪碱在5.868～293.4 mg·L-1范围内,与色谱峰峰面积呈良好线性关系,相关系数为0.9999,平均加样回收率为100.7%,RSD为0.8%(n=6).结论:对氢溴酸东莨菪碱的含量及降解产物进行研究表明,方法简便、快速,结果准确、专属性强.     

Application of potassium dichromate and iron-thiocyanate in the spectrophotometric investigations of phenothiazines

A spectrophotometric procedure for the determination of phenothiazines in pure form and in a number of their pharmaceutical preparations has been developed that offers the advantages of simplicity, accuracy, precision and sensitivity over many other methods. The method is based on the oxidation of phenothiazines by a known excess amount of potassium dichromate followed by the estimation of unreacted amount of dichromate by reacting with excess of iron(II) and measuring the iron(III) formed by complexing with thiocyanate. The reacted oxidant corresponds to the drug content. Different variables affecting the reaction between drugs and dichromate were studied and optimized. At the maximum absorption of 480 nm, Beer's law is obeyed in the range 2.5-29.75 microg/ml. The molar absorptivity and Sandell sensitivity of the procedure were calculated in addition to detection limit. Statistical treatment of the experimental results indicates that the procedure is precise and accurate. Excipients used as additives in pharmaceutical formulations did not interfere in the proposed procedure. The reliability of the method was established by parallel determination against the official BP methods. The procedure described was successfully applied to the determination of the bulk drugs and in pharmaceutical formulations.     

前胡类药材的化学成分及质量控制方法研究

目的：概述前胡类药材化学成分及其相关成方制剂的质量控制标准的研究现状,为前胡类药材及成药的标准研究提供参考。方法：检索并查阅前胡类药材相关研究文献及标准记载情况,归纳其主要化学成分及制剂的质量控制方法。结果：以“前胡”为药材名的药用植物较多,其所含化学成分主要有香豆素类、黄酮类、萜类及挥发油类;质量标准除《中华人民共和国药典》收载前胡及紫花前胡外,尚有多省份地方药材标准收载以前胡的近缘种作为地方习用品使用。质量控制方法主要涉及性状鉴别、显微鉴别、薄层鉴别、指纹图谱、含量测定等方法。结论：前胡为常用传统中药,应用广泛,前胡及其中成药的质量标准参差不齐,有待进一步提升。     

Investigation on the marker substances of crude drugs in formulations. I. Marker substances for the identification of astragali radix in kampo and drinkable preparations]

There are few reports about marker substances for the identification of Astragali Radix in formulations. First, constituents analysis was performed by HPLC for the screening of a marker substance, using several lots of Astragali Radix and its fluid extracts. As a result of the analysis, one of the main components was clearly detected even in the fluid extracts, and thought to be a good marker substance. This component was identified to be calycosin (7,3'-dihydroxy-4'-methoxyisoflavone) by the structural analysis. Then, the identification methods of Astragali Radix and its fluid extracts in formulations were investigated with an Astragali Radix extract as a reference standard solution and calycosin as a marker substance. This method was applied to three different kinds of Kampo formulations and three different kinds of drinkable preparations. Consequently, calycosin was clearly detected by a HPLC-multi wavelength detector system, in all investigated formulations. Calycosin will be successfully used as a marker substance for the identification of Astragali Radix and its fluid extracts in formulations.     

齐墩果酸含量测定的研究进展

齐墩果酸是多种中药的有效成分之一,具有多方面的重要生物活性,许多中药及其制剂均选用齐墩果酸的含量作为其质量控制的指标,本文对齐墩果酸含量测定方法的研究进展作一综述。随着含齐墩果酸中药的指纹图谱和质量标准方面研究的不断发展,简便快速、准确高效的测定方法也将会不断涌现,齐墩果酸的分离和含量测定技术将会日臻完善,为制剂中齐墩果酸的质量控制提供更可靠的依据。     

Investigation on the marker substances of crude drugs in formulations. II. Marker substances for the identification of Cistanchis Herba in drinkable preparations

There are few reports about marker substances for the identification of Cistanchis Herba in formulations. First, constituent analysis was performed by HPLC for screening of a marker substance, using several lots of Cistanchis Herba and its fluid extract. As a result, two components were clearly detected, which were thought to be good marker substances and identified to be echinacoside and acteoside by structural analysis. Stability testing of these two marker substances in various pH and temperature conditions was carried out, which suggested that they are stable and suitable enough for the identification. Therefore, the identification methods of Cistanchis Herba and its fluid extract in formulations were investigated using five different kinds of commercial drinkable preparations with authentic standard of echinacoside and acteoside as marker substances. Consequently, echinacoside and acteoside were clearly detected in all formulations investigated, using an HPLC-photodiode array detector system. Echinacoside and acteoside will be successfully used as marker substances for the identification of Cistanchis Herba and its fluid extract in formulations.     

Formulation of medicines for children

The development of age-adapted dosage forms and taste-masking of bitter-tasting drugs administered orally for children, are formidable challenges for formulation scientists. Childhood is a period of maturation requiring knowledge of developmental pharmacology to establish dose but the ability of the child to manage different dosage forms and devices also changes. Paediatric formulations must allow accurate administration of the dose to children of widely varying age and weight. Whilst the oral route will be preferred for long term use and the intravenous route for the acutely ill, many of the dosage forms designed for adults, such as oro-dispersible tablets, buccal gels and transdermal patches, would also benefit children if they contained an appropriate paediatric dose. The age at which children can swallow conventional tablets is of great importance for their safety. Liquid medicines are usually recommended for infants and younger dhildren so the ability to mask unpleasant taste with sweeteners and flavours is crucial. More sophisticated formulations such as granules and oro-dispersible tablets may be required but there will be limitations on choice and concentration of excipients. There are many gaps in our knowledge about paediatric formulations and many challenges for the industry if suitable preparations are to be available for all ranges. A CHMP points to consider document is soon to be released. More research and clinical feedback are important because a formulation with poor acceptability may affect compliance, prescribing practice and ultimately commercial viability.     

Comparison of capillary zone electrophoresis and high performance liquid chromatography methods for quantitative determination of ketoconazole in drug formulations

A capillary zone electrophoresis (CZE) and a high-performance liquid chromatography (HPLC) method have been developed for identification and determination of ketoconazole, an imidazole antifungal, in pharmaceutical preparations. The suitabilities of both methods for quantitative determination of ketoconazole were approved through validation specification such as linearity, precision, accuracy, limit of detection and quantification. The proposed methods were used for determination of ketoconazole in commercial pharmaceutical dosage forms (tablets and creams). Under described conditions, CZE method is more selective, while the HPLC method is more sensitive. Both methods are rapid (tR(CZE)=5.14 min and tR(HPLC)=2.66 min), which is important for routine application. However, the HPLC method provides a repeatability of the quantitative analysis of ketoconazole in drug formulations below 1.5% relative standard deviation (R.S.D), while the repeatability of the CZE method is in the order of 2-3% R.S.D.     

Colorimetric acetaminophen determination in pharmaceutical formulations.

Different approaches for the colorimetric determination of acetaminophen, based on its coupling with diazotized o-nitroaniline, are described. Copper(II) chelation with the coupled compound makes the method highly selective. Sensitivity is increased when the acetaminophen assay is carried out indirectly through the determination of the chelate's copper content. Optimum conditions for performing the different approaches are described. The stoichiometric balance for the reactants in the coupled compound and chelate is determined. The degree of dissociation and the instability constant are computed. The rectilinear relationship between the absorbance of the different products and the concentration of acetaminophen allows for its determination in different pharmaceutical formulations. Compared with the official method, the proposed methods give more accurate results.     

基于大生产考察烫制对骨碎补中柚皮苷含量的影响

目的考察烫制对骨碎补中柚皮苷含量的影响及其影响因素。方法建立烫骨碎补中柚皮苷含量的高效液相色谱法。实地参与中药饮片生产企业烫骨碎补的砂烫炮制过程,考察不同温度、炮制时长对柚皮苷含量的影响,并测定不同企业的多批次骨碎补药材及相对应的烫骨碎补饮片中柚皮苷的含量。结果柚皮苷进样量线性范围为3. 561 2~2 226 ng(r=0. 999 9),精密度、稳定性、重复性试验的RSD均小于3. 0%,平均加样回收率为99. 58%,RSD为1. 31%(n=9)。随着炮制时间的延长,柚皮苷含量逐渐降低,且受烫制温度影响。收集的10批次烫骨碎补与烫制前相比,柚皮苷含量4批次明显升高,2批次明显降低,4批次未见明显变化。结论建立含量测定的方法简便、准确,可用于测定烫骨碎补柚皮苷的含量。烫制时温度、时长及原料规格均一性是影响柚皮苷含量的关键因素。