胃舒散质控方法中含铋量标准的校正及秩和检验

目的 :校正胃舒散含铋量标准。方法 :采用络合滴定法测定胃舒散以及3个对照品中有效铋的含量 ,并对胃舒散调整剂量后进行临床秩和检验。结果 :通过比较 ,胃舒散原来的含铋量较高。胃舒散中碱式碳酸铋投料量在处方工艺条件下减半为7 0kg。结论 :质量标准修订为每1 0g胃舒散含碱式碳酸铋0 10g(±10% )。     

阿育魏实挥发油的提取工艺研究

目的比较研究微波萃取法和索氏提取法对阿育魏实挥发油的提取工艺。方法以得油率为指标,液料比、蒸馏时间、提取时间、碎粒度为提取因素进行正交试验得出最佳工艺。结果索氏提取法当取样量为20 g、提取时间为4 h、碎粒度为粉碎状、虹吸速度为中速时为最佳提取条件;而微波法当取样量为25 g、微波时间为90 s、浸泡时间为30 min、碎粒度为粉碎状,即为最佳提取条件。结论与索氏法比较,微波法节约能耗,提取速率快,适合大量快速提取。     

正交试验优化人参的微波灭菌工艺研究

目的 优选人参药材微波灭菌工艺.方法 以灭菌率为指标,采用正交试验对药材粒度、灭菌时间、灭菌功率进行考察,并考察微波灭菌对人参皂苷的影响.结果 筛选出最佳微波灭菌工艺:灭菌时间240 s、人参药材粒度为细粉(10目)、灭菌功率6 000 W.结论 优选的工艺灭菌效率高,简便可行.     

莪术挥发油提取工艺的研究

目的利用正交设计优选法确定提取莪术挥发油的最佳工艺条件。方法以莪术油的含量为指标,通过L9(34)正交试验设计,对提取工艺中的浸泡时间、提取时间、加水量和药材粒度4个因素进行优选研究,以筛选出莪术挥发油的最佳提取工艺条件。结果影响提取的主次因素为:提取时间>药材粒度>浸泡时间>加水量。优选得到的最佳提取工艺条件是浸泡12h,提取5h,加水7倍,药材粒度为粒状。结论本工艺条件科学合理,稳定可行,可有效保证产品质量。     

正交试验优化杏贝止咳提取物的微波干燥工艺

目的优化杏贝止咳提取物的微波干燥工艺参数。方法以苦杏仁苷、白花前胡甲素和白花前胡乙素综合转移率为考察指标,选取微波功率、干燥时间、铺盘厚度、真空度作为优化试验考察因素,每个因素设计3个水平,采用L9(34)正交试验优化杏贝止咳浸膏的微波干燥工艺,并与常规干燥工艺进行比较。结果杏贝止咳浸膏最佳微波干燥工艺为微波功率6k W,干燥时间9 min,铺盘厚度2~2.5 cm,真空度-0.08~-0.09 MPa。结论该工艺高效节能,稳定可行,为改善杏贝止咳颗粒的干燥工艺提供实验依据。     

Box-Behnken响应面法优化升降茶制备工艺研究

摘要：目的:通过研究不同关键参数对茶剂质量的影响,优化升降茶的制备工艺。方法:采用Box-Behnken响应面法,以药粉细度(目)、润湿剂用量(倍)、干燥温度(℃)、干燥时间(h)为关键影响参数,计算成型率(%)、休止角(度)和吸湿率(%),评估总评OD值以反映质量属性,建立关键影响参数与质量属性之间的数学模型,并选取优化后的空间点进行质量验证。结果:经过Design-Expert10.0软件模型回归和响应面分析,确定较优制备升降茶的工艺操作工艺为：药粉细度60目,润湿剂用量1倍,干燥温度为70℃、干燥时间4 h。3次验证试验RSD均小于2%。结论:Box-Behnken效应面法可用于升降茶制备工艺的优化,且所确定的工艺参数简便易行,稳定可控,可进行产业化生产。     

不同工艺干燥的玄参中安格洛苷-C的含量分析

目的:探讨干燥工艺对玄参质量的影响,分析不同工艺干燥的玄参中安格洛苷-C的含量。方法:将鲜玄参分别采用自然晾晒和微波真空干燥,采用高效液相色谱法,分析不同工艺干燥玄参中安格洛苷-C的含量。色谱条件为Kromasil C-18色谱柱(250mm×4.6mm,5μm),流动相:甲醇-乙腈-1%冰醋酸溶液,梯度洗脱,流速:1ml/min,检测波长:276nm,柱温:25℃。结果:两种干燥方法玄参中安格洛苷-C与其它的成分能达到很好的分离,微波真空干燥玄参的安格洛苷-C含量高于自然晾晒干燥玄参的含量。结论:微波真空干燥技术用于中药玄参的干燥,不仅工艺简单、干燥时间短,而且安格洛苷-C有效成分有较高的保留。     

辛白鼻渊颗粒喷雾制粒工艺优选

目的优选辛白鼻渊颗粒喷雾制粒的最佳工艺。方法采用正交试验法,以喷雾干燥后药粉产量为考察指标优选工艺条件,并进行验证试验和成品质量考察。结果最佳工艺参数为进风温度90℃,喷液转速6 r/min,风机频率45 Hz;薄层鉴别结果显示,供试品溶液色谱中,在与黄芩苷和栀子苷对照品溶液色谱相应位置上显相同颜色的斑点;成品颗粒的主要成分、流动性、粒度、水分、干燥失重和溶化性检查均符合2015年版《中国药典(四部)》规定。结论优选制备工艺所制得的颗粒质量稳定,产品收率高,适宜于工业化生产。     

正交设计优选苦参微波提取工艺

目的 优选苦参微波提取法的最佳工艺条件.方法 以苦参碱、苦参总碱和干浸膏得率为指标综合评判,采用L9(34)正交试验法,优选苦参微波提取的工艺条件.结果 优化微波提取法工艺条件为三煎固液比依次为6倍、4倍、4倍,药材粒度为10 ～ 20目,煎煮总时间为3 min,三煎依次为2,0.5,0.5 min,辐射频率为600 Hz.结论 该工艺科学合理,有利于综合考察苦参药效物质的提取效果.     

正交试验优选愈肝宁贴剂制备工艺

目的:优选愈肝宁贴剂的制备工艺。方法:以用膏量、固化时间、干燥温度、干燥时间为考察因素,以初黏力、剥离强度和皮肤残留现象为指标,用正交试验法优选出最佳制备工艺。结果:以用膏量(7.6±0.1)g·100cm-2、固化时间24h、干燥温度60℃、干燥时间3.5h为最佳制备工艺,并符合质量控制方法。结论:优选的最佳工艺方案可行,所制备的愈肝宁贴剂质量稳定。     

微波技术在试样干燥失重分析中的应用

目的：将微波技术用于试样干燥失重的测定。方法：分别对扑热息痛、硫酸奎宁、无水碳酸钠、硫酸钙等含有自由水和结合不的有机和无机药品的微波功率、干燥时间及试样数量与燥失重率的关系进行研究。结果：本法结果准确,精密度高,各 试吕均可在１０ｍｉｎ内完成测定,与烘箱汉比较,节省能源９５％以上,提高工作效率１５倍以上。结论：本法适用于化学药品干燥失重的常规分析。     

不同干燥方式对中药提取物粉体学性质的影响

目的：考察不同干燥方式对复方中药舒胸片方提取物粉体学性质的影响。方法以真空干燥、微波真空干燥及喷雾干燥三种方法,探讨不同干燥方式对复方中药舒胸片方提取物粉体学性质的差异。结果三者中真空干燥产物流动性最好,微波真空干燥产物的平衡吸湿量最小,喷雾干燥所得圆整性好、粒匀,压缩成型性较优。结论干燥工艺不同导致了干燥产物粉体学性质的差异,各粉体学性质之间存在一定的相关性。     

Microwave-assisted drying of pharmaceutical granules and its impact on drug stability

The advent of microwave technology has intensified the search for pharmaceuticals amenable to microwave processing. This study investigated the influences of powder load, diluent particle size and amount of granulating liquid employed on the microwave-assisted drying and stability of acetylsalicylic acid (ASA)-loaded granules in a single pot high shear processor. Powder load affected the profiles, rate and extent of drying. Drying was more dependent on the size and structural properties of granules rather than their surface areas as heat was generated volumetrically. Increased granule size brought about by increasing the size of diluent particles and amount of granulating liquid resulted in higher drying rates. Drug stability was negatively correlated to the drying time of granules.     

Process design applied to optimise a directly compressible powder produced via a continuous manufacturing process.

Manufacturing of 'ready-to-compress' powder mixtures for direct compression was performed by spray drying, without granulation, milling and/or blending steps in between spray drying and compaction. Powder mixtures containing acetaminophen, mannitol, erythritol, maltodextrin, crospovidone, colloidal silicon dioxide and polyoxyethylene 20 sorbitan monooleate were prepared via co-spray drying. A feed suspension having a solid content of 27.2% w/w was selected for further process optimisation because of its high process yield, excellent flowability and short tablet disintegration time. Experimental design was applied to evaluate processibility, physico-chemical properties and compactability of the spray dried powder mixtures. Significant and adequate regression models were developed for powder flowability, median particle size, bulk density, residual moisture content and process yield. An increasing inlet and outlet drying air temperature improved process yield. However, a higher inlet drying air temperature had a negative influence on density and moisture content, while the latter decreased at higher outlet drying air temperatures. Median particle size increased with a higher inlet temperature, while the outlet temperature had the opposite affect. Numerical optimisation determined the optimal spray drying process (inlet temperature: 221 degrees C, outlet temperature: 81 degrees C and atomisation pressure: 6 bar) in order to produce 'ready-to-compress' powder mixtures.     

红外光谱和高效液相指纹图谱用于安多霖不同干燥工艺的评价研究

目的建立安多霖胶囊内容物的红外光谱和HPLC指纹图谱,考察喷雾干燥与微波干燥对安多霖胶囊内容物的影响。方法分别对安多霖配方提取液选择喷雾干燥、微波干燥两种方法,制备8批供试品,绘制8批粉体的红外光谱图,采用高效液相色谱法,梯度洗脱绘制不同粉体溶液的HPLC指纹图谱,比较不同干燥方法所得粉体的图谱,评价不同干燥工艺的优劣。结果安多霖胶囊配方提取液经喷雾干燥和微波干燥后,其红外光谱和HPLC指纹图谱极其相似,不同干燥工艺没有引起安多霖胶囊物质基础的改变。结论不同干燥工艺所得安多霖胶囊内容物的物质种类和总量极其相似,两种干燥方法均可应用于安多霖胶囊配方提取液的干燥。     

Spray drying of fenofibrate loaded nanostructured lipid carriers

The conversion of aqueous dispersion of nanostructured lipid carriers (NLCs) into dry powder by spray drying could be a useful approach to render NLCs with better physical chemical stability than the aqueous dispersion. In this study, aqueous NLC dispersion containing fenofibrate was converted into dry, easily reconstitutable powder using spray drying. A central composite face centered design (CCFD) was used to investigate the influence of the ratio of lipid to protectant (mannitol and trehalose) and crystallinity of spray-dried powder on the particle size, yield and residual moisture content of the dried powder. A linear relationship (R² = 0.9915) was established between the crystalline content of the spray-dried powders against the ratio of mannitol to trehalose from 3:7 to 10:0 (w/w). Spray drying of NLC aqueous dispersion using a mannitol and trehalose mixture resulted in an increase in particle size of the NLCs after reconstitution in water as compared to that in the initial aqueous dispersion. The decrease in crystallinity of the dry powder by reducing the ratio of mannitol to trehalose could improve the reconstitution of the NLCs in water. However the yield and residual moisture content of dry powder decreased with an increase in the ratio of mannitol to trehalose. Lipid nanoparticles were able to retain the drug incorporation and the prolonged drug release profile after spray drying. The experimental model was robust, and suggested that spray drying is a viable technique for the conversion of NLCs into dry powder.     

Benefit of microwaves in case of heat-sensitive agglomerate drying

The microwave assisted vacuum drying of heat-sensitive materials is increasing in the pharmaceutical industry since the eighties. This paper deals with results of two experiment series obtained on a laboratory scale single pot dryer (Collette Ultima 251). Firstly water was heated up to the boiling point exclusively by predetermined microwave energy and then by various wall temperatures in order to determine the convection efficiency of the system. The experiments were carried out at fixed pressure level (80 mbar) and with optimum bowl load (15 kg). According to the demonstrated idea each single pot system efficiency can be specified at any type and quantity of load. With the help of the presented results the second experiments were designed to compare the microwave and convection efficiency of the single pot system during granule drying. A placebo granule was dried either by an exclusive convection or microwave method up to the determined LOD (< 0.5%). According to the tests extreme high wall temperature (85 degrees C) had to be used to achieve the same drying time--and efficiency--as with the usage of dielectric heating. Based on the results it can be stated that the shorter drying time under favourable conditions is the advantage of microwave radiation over the conventional technique.     

微波技术对黄芩中黄芩苷浸出量影响的研究

目的：研究微波技术对黄芩中黄芩苷浸出量的影响。方法：对不同浸出方法。药材粒径,浸出时间及微波输出功率进行正交试验。优选黄芩中黄芩苷最佳浸出方案;用紫外分光光度法对黄芩浸出液中黄芩苷含量进行测定。结果：微波技术对黄芩中黄芩苷的浸入量明显优于常规煎煮方法。结论：微波技术应用于药材浸出是一种省时便捷,值得推广普及的中药浸出新方法;半量黄芩粗粉的浸出量优于全量黄芩饮片的浸出量,与中医药理论“煮散减半”相符。     

正交优化鬼针草总生物碱的微波萃取工艺

目的:微波萃取法优化鬼针草总生物碱提取条件。方法:采用正交试验L9(34)法对鬼针草总生物碱的微波萃取条件进行优化设计。结果:鬼针草总生物碱的最佳提取条件为A3B3C2D1的组合,溶剂体积分数对萃取影响较大。结论:优选的提取条件效率高,可增加鬼针草的利用率。     

螺旋霉素超细粉的喷干法和反溶剂法制备及性质研究

摘要：目的 螺旋霉素原料药粉的粒径大、团聚现象严重,因此极大的限制了其临床应用;有研究报道超细粉制备技术可 以很好地解决这些问题; 方法 采用了两种代表性的方法制备螺旋霉素的超细粉：分别为喷雾干燥法和反溶剂法;并以粒径为 指标,采用单因素实验优化得到最佳结果,对上述两种方法制备的粉体分别进行粒径、形貌特征和物化性质对比。结果 两种 方法的最佳条件为：喷雾干燥法的进料速度为5 mL/min,雾化空气速度为800 L/h,进口温度为150℃,出口温度为85℃,平均 粒径为(1638±10.99) nm。反溶剂法在25℃条件进行实验,溶剂与反溶剂的比例为1:5,最佳搅拌速度为1000 r/min,获得的平均 粒径为(230±7.31)nm,以上结果经过扫描电子显微镜(SEM),动态光散射(DLS),傅立叶变换红外光谱(FTIR),差示扫描量热仪 (DSC)和X射线衍射(XRD)进行表征;经气相色谱检测,两种方法中的溶剂残留均符合ICH最低标准(5000 ppm);结论 与喷雾干 燥法相比,反溶剂法制备的螺旋霉素粒径更小、粉体分散性更佳,其溶解度更高。因此反溶剂法制备的螺旋酶素微粉更适用于 制药业,为微粉技术提供技术思路。