盐酸小檗碱片微生物限度检查方法验证浅析

分析进行盐酸小檗碱片微生物限度检查方法验证实验的必要性.按<中国药典>2005版规定,对7个生产企业生产的盐酸小檗碱片进行微生物限度检查方法的验证.盐酸小檗碱对5株阳性代表菌株有不同程度的抗菌活性,不同厂家的产品的抗菌活性类似.可建立统一的盐酸小檗碱片的微生物限度检查方法.     

关于盐酸小檗碱片溶出度检查的商榷

目的　探讨盐酸小檗碱片的溶出度检查。方法　以盐酸小檗碱片溶出度检查给定的吸收系数及样品液浓度 ( 8mg·L-1) ,设计用紫外分光光度法测定盐酸小檗碱片的含量 ,并与药典法进行了比较 ;同时测定了 2个厂家 4个批号盐酸小檗碱片的溶出度及其含量。结果与结论　紫外分光光度法不适用于盐酸小檗碱片的含量测定 ;此法用于盐酸小檗碱片溶出度检查时溶出量限度 Q值定得偏高     

治痢片体外抗菌实验

目的：观察治痢片及盐酸小檗碱的体外抗菌作用及盐酸小檗碱和空白（治痢片中盐酸碱小檗碱以外的药物）的交互作用对治疗痢片抗菌作用的影响。方法：采用液体两倍稀释法和药物交互作用定量法。结果：治痢片和盐酸小檗碱对金黄色葡萄球菌具有很强的抗菌作用。在所选用的痢疾杆菌中，治痢片对痢疾志贺菌Ⅱ型的抗菌作用最强。盐酸小壁碱与空白的交互作用导致治痢片抗菌作用降低。结论：增加治痢片中盐酸小檗碱的含量，对空白应进行有效成分提取、精制，再做成缓释剂以降低对盐酸小檗碱的干扰，可提高治痢片抗菌效果。     

复方黄连素片中盐酸小檗碱含量测定方法改进

目的改进复方黄连素片中盐酸小檗碱的含量测定方法。方法采用高效液相色谱法测定复方黄连素片中盐酸小檗碱的含量。结果改进的方法简便、准确、重现性好。结论所拟订的方法可对复方黄连素片中的盐酸小檗碱含量测定方法的改进提供参考依据。     

盐酸小檗碱原料药及其片剂杂质鉴定及分析方法建立

目的：探讨植物来源盐酸小檗碱及其片剂主要杂质并鉴定未知杂质化学结构,建立有关物质分析方法,为《中国药典》2020年版盐酸小檗碱及盐酸小檗碱片有关物质分析方法的修订/增加提供参考。方法：采用LC-MS对盐酸小檗碱中主要未知杂质进行鉴定,优化《中国药典》2020年版盐酸小檗碱有关物质项下分析方法,并进行验证,同时测定多批次原料药及片剂有关物质的含量。结果：除《中国药典》2020年版盐酸小檗碱有关物质项下规定的已知杂质盐酸药根碱、盐酸巴马汀外,首次鉴定出其余3个含量超出鉴定限（0.1%）的未知杂质去亚甲基小檗碱、小檗红碱、芬氏唐松草定碱;建立可同时测定去亚甲基小檗碱、小檗红碱、芬氏唐松草定碱、盐酸药根碱、盐酸巴马汀的高效液相色谱法,经方法学验证,系统适用性、专属性、线性、检测限、定量限、重复性、中间精密度、准确度、耐用性均符合要求,并完成多批次样品检测。结论：在现行《中国药典》2020年版盐酸小檗碱的有关物质测定方法及限度要求基础上,优化色谱条件,同时增加对已知杂质的控制限度,更好的对盐酸小檗碱及盐酸小檗碱片进行质量控制。     

改进盐酸小檗碱片含量测定方法的探讨

目的;测定盐酸小檗碱片的含量.方法:采用改进药典法.结果:经统计分析,与药典法比较无显著性差异(P＞0.05),且操作方便、误差小.结论:改进药典法可作为测定盐酸小檗碱片含量的方法.     

关于盐酸小檗碱片含量测定的探讨

目的对于盐酸小檗碱片的含量测定中的一些问题进行探讨。方法采用讨论、比较的方式,提出问题,并讨论解决问题的方法。结果盐酸小檗碱片有多种分析方法,各有优点及不足,结论应尽快找到更加完善的测量盐酸小檗碱的方法,以弥补现行标准的不足。     

分光光度法鉴别盐酸小檗碱片的掺假

盐酸小檗碱系天然广谱抗菌药,对痢疾杆菌等的肠道感染有独特的疗效。《中国药典》2000年版二部收载盐酸小檗碱片,其含量测定的原理是根据盐酸小檗碱能被重铬酸钾氧化成酸、醛及去氢小檗碱,过量重铬酸钾用硫代硫酸钠滴定液回滴测定含量。溶出度测定是根据盐酸小檗碱在263nm处有最大     

三黄片的真伪优劣鉴别

目的 建立中成药三黄片真伪优劣的鉴别方法.方法 采用TLC法、HPLC-MS法及HPLC指纹图谱法,确定方中的盐酸小檗碱是否有减量投料或以药材替代投料的情况.结果 所建立的TLC法可初步判定盐酸小檗碱是否减量投料或以药材替代投料,HPLC-MS鉴别和HPLC指纹图谱测定可确定盐酸小檗碱是否有减量投料或以药材替代投料的情况发生.结论 该方法专属性强、准确可靠,能快速鉴别三黄片的真伪优劣.     

结肠靶向制剂盐酸小檗碱控释片的稳定性考察

目的考察自制结肠靶向制剂盐酸小檗碱控释片的稳定性。方法自制盐酸小檗碱包衣片在光照、高热、高湿条件下露置,并做加速实验及室温留样实验,定时取样,测定盐酸小檗碱的含量及片剂的溶出度。结果盐酸小檗碱片在光照、高热、高湿下均稳定,含量基本不变,高温条件下溶出度变小,其它各项指标均未发生明显改变,加速实验及室温留样,其各项指标也未发生明显改变,可暂定有效期为2年。结论盐酸小檗碱片对光、热、湿均不敏感,有效期为两年。     

利巴韦林片的处方优化

目的：筛选利巴韦林片的最佳处方。方法：考察糊精、羧甲基淀粉钠、微晶纤维素和低取代羟丙基纤维素对利巴韦林片的质量影响。结果：所筛选的适宜润湿剂为75％乙醇，L－HPC和微晶纤维素的最佳用量分别为10％和15％。按照最佳处方制备的利巴韦林片硬度和外观大为改善。结论：本法处方合理，工艺简单，所制备的利巴韦林片适合临床应用。     

银黄酮片的处方优化

目的 :筛选银黄酮片的最佳处方。方法 :考察糊精、羧甲基淀粉钠、微晶纤维素和低取代羟丙基纤维素对银黄酮片的质量影响。结果 :筛选的最佳处方为5 %低取代羟丙基纤维素。按照最佳处方制备的银黄酮片崩解度大为提高。结论 :本法处方合理 ,工艺简单 ,所制备的银黄酮片适合临床应用。     

Influence of different types of low substituted hydroxypropyl cellulose on tableting,disintegration, and floating behaviour of floating drug delivery systems

The object of the present study is to evaluate the effect of application of low-substituted hydroxypropyl cellulose (L-HPC) 11 and B1 as excipients promoting floating in gastroretentive tablets. Directly compressed tablets were formed based on experimental design. Face-centred central composite design was applied with two factors and 3 levels, where amount of sodium alginate (X₁) and L-HPC (X₂) were the numerical factors. Applied types of L-HPCs and their 1:1 mixture were included in a categorical factor (X₃). Studied parameters were floating lag time, floating time, floating force, swelling behaviour of tablets and dissolution of paracetamol, which was used as a model active substance. Due to their physical character, L-HPCs had different water uptake and flowability. Lower flowability and lower water uptake was observed after 60 min at L-HPC 11 compared to L-HPC B1. Shorter floating times were detected at L-HPC 11 and L-HPC mixtures with 0.5% content of sodium alginate, whereas alginate was the only significant factor. Evaluating results of drug release and swelling studies on floating tablets revealed correlation, which can serve to help to understand the mechanism of action of L-HPCs in the field development of gastroretentive dosage forms.     

In vitro evaluation of micronized low-substituted hydroxypropylcellulose as an insoluble swellable matrix for sustained-release tablets.

Micronized low-substituted hydroxypropylcellulose (L-HPC) was evaluated in vitro as an insoluble swellable matrix carrier for sustained-release tablets, using procainamide hydrochloride, theophylline and indomethacin. The amount of water-soluble fraction and the degree of aggregation of L-HPC particles in water increased with decreases in the particle size. The mechanisms of formation of non-disintegrating matrix tablets by micronized L-HPC are discussed on the basis of fast hydration and gel formation due to loss of the fibrous structural integrity of the cellulose polymer. Simple power law analysis suggests that the drug release from directly compressed L-HPC matrices is affected not only by polymer swelling but also by the drug solubility and the amount of soluble fraction in the matrices.     

小儿清热止咳分散片的填充剂与崩解剂筛选

目的为了制备中药分散片,以小儿清热止咳糖浆方剂为模型药物筛选中药分散片的填充剂和崩解剂。方法以抗张强度、吸湿性和压缩功作为选择填充剂的依据,以吸水性实验、溶胀度实验、空白片崩解时限和加入质量分数为50%浸膏的片剂崩解时限为选择崩解剂的依据。测定发泡量和产气量作为选择泡腾崩解剂的依据。结果综合以抗张强度、吸湿性和压缩功大小,选择乳糖作为分散片的填充剂。溶胀性能优劣顺序是:CMS-Na>L-HPC(信越)>PVPP>MCC101>MCC301>L-HPC(国产)>MCC302>MCC102>滑石粉>干淀粉;吸水性能优劣顺序是:L-HPC(信越)>L-HPC(国产)>CMS-Na>PVPP>MCC302>MCC102>MCC301>MCC101>浸膏;单独使用微晶纤维素或超级崩解剂达不到分散片的质量要求,联用微晶纤维素和超级崩解剂,可以达到分散片质量要求。结论中药分散片的崩解剂可以采用超级崩解剂和微晶纤维素的混合物,泡腾崩解剂选用酒石酸和碳酸氢钠,其摩尔比为1.0∶0.8。     

单硝酸异山梨酯口腔崩解片的制备及药剂学研究

目的:筛选单硝酸异山梨酯口腔崩解片的处方并考察片剂质量。方法:采用正交设计法筛选片剂处方,用HPLC法测定片剂的含量。结果:所得的优化处方为:MCC与L-HPC的比例为8:2(32%,8%),CC- Na为3%,甘露醇为15%,乳糖为31%。所得的片剂在20 s内完全崩解,1 min释药80%以上,口感良好。结论:选择合适的辅料,可以生产出崩解快、口感好,能够快速起效的口腔崩解片。     

红景天分散片的研制及质量控制

目的：探讨红景天分散片制备工艺及质量标准。方法：采用正交设计法对红景天分散片的辅料进行了筛选，并对质量控制方法进行了研究。结果：选择2％低取代羟丙基纤维素（L-HPC）、10％羧甲基淀粉钠（CMS—Na）为崩解剂，2％聚乙烯吡咯烷酮（PVPK-30）的20％乙醇溶液为黏合剂，0．2％硬脂酸镁为润滑剂，进行湿法制粒压片。制备的分散片每片含红景天多糖0．1g，崩解时限为35s，45min溶出量为标示量的76．73％，符合中华人民共和国药典（2005年版）对分散片的要求。结论：所制备的红景天分散片制备工艺简单，溶出度高，性质稳定，具有实用价值。     

复方双参口腔崩解片的制备工艺研究

目的：制备复方双参口腔崩解片,使用星点设计-效应面优化法对处方工艺进行优化筛选。方法：以丹参水提物和人参皂苷为主药,采用粉末直接压片法制备复方双参口腔崩解片,选择MCC／L—HPC（8：2）和PVPP作为联合崩解剂。以MCC／L—HPC的用量及PVPP的用量为考察因素,崩解时限作为评价指标,用线性方程和二次及三次多项式描述崩解时限和两个影响因素之间的数学关系,根据最佳数学模型描绘效应面及等高线图,选择最佳处方,并进行预测分析。结果：当MCC／L—HPC含量25％,PVPP含量8．2％时,片剂的崩解时间最短。各指标的三项式拟合方程均优于多元线形回归方程,建立的数学模型的预测值与实际值符合较好。结论：用星点设计-效应面法优化复方双参口腔崩解片处方工艺预测性良好。     

Preformulation studies and optimization of sodium alginate based floating drug delivery system for eradication of Helicobacter pylori

The aim of this study was to design a local, floating, mucoadhesive drug delivery system containing metronidazole for Helicobacter pylori eradication. Face-centered central composite design (with three factors, in three levels) was used for evaluation and optimization of in vitro floating and dissolution studies. Sodium alginate (X₁), low substituted hydroxypropyl cellulose (L-HPC B1, X₂) and sodium bicarbonate (X₃) concentrations were the independent variables in the development of effervescent floating tablets. All tablets showed acceptable physicochemical properties. Statistical analysis revealed that tablets with 5.00% sodium alginate, 38.63% L-HPC B1 and 8.45% sodium bicarbonate content showed promising in vitro floating and dissolution properties for further examinations. Optimized floating tablets expressed remarkable floating force. Their in vitro dissolution studies were compared with two commercially available non-floating metronidazole products and then microbiologically detected dissolution, ex vivo detachment force, rheological mucoadhesion studies and compatibility studies were carried out. Remarkable similarity (f₁, f₂) between in vitro spectrophotometrically and microbiologically detected dissolutions was found. Studies revealed significant ex vivo mucoadhesion of optimized tablets, which was considerably increased by L-HPC. In vivo X-ray CT studies of optimized tablets showed 8 h gastroretention in rats represented by an animation prepared by special CT technique.     

雷公藤多苷分散片的制备工艺研究及质量控制

目的制备雷公藤多苷分散片。方法筛选崩解剂、润湿剂、制粒方法、颗粒压片条件,并控制其质量。结果崩解剂的最佳比例为MCC：L-HPC=11：3;制粒时选用水为其润湿剂,润湿剂用量为药粉重量的80%（ml/g）;20目筛制粒,30目筛整粒。所制备的分散片在3min内崩解完全,含量均匀,稳定性好,符合分散片的各项指标。结论本品达到分散片的要求,制剂稳定。