中国药典2015年版尿素含量测定结果影响因素的探讨

目的：考察干燥失重检查项对尿素含量测定结果的影响,为药品质量控制提供参考。方法:用《中国药典》2015年版二部方法对尿素含量进行测定,用《中国药典》2015年版四部通则0831干燥失重测定法测定干燥失重,并对测定结果进行了比较分析。结果:按干燥品计算的测定结果高于原标准测定结果。结论: 建议增加干燥失重检查项,含量按干燥品计算,现行检验标准有待修改。     

关于《中国药典》2005年版二部“干燥失重测定法”中对减压干燥新增温度规定的若干思考

在《中国药典》2000年版中，当测定颗粒剂的【干燥失重】时规定：“除另有规定外，照干燥失重测定法测定，含糖颗粒剂宜在80℃真空干燥，减失重量不得超过2．0％”。但附录“干燥失重测定法”中并未规定干燥温度。为消除此缺陷，2005年版药典在颗粒剂【干燥失重】测定中增加了温度的规定：“…于105℃干燥至恒重”。[第一段]     

氨磷汀水分测定方法比较

目的：比较干燥失重法、卡氏法、减压干燥法、甲苯法四种方法测定氨磷汀结晶水含量的效果。方法：分别用上述四种方法测定氨磷汀结晶水含量,并对结果进行比较。结果：氨磷汀样品不能采用干燥失重法测定水分。80℃减压干燥法,虽然干燥前后样品有关物质没有明显变化,但12h之内并不能完全将结晶水从样品中分离出来。甲苯法所需求的样品量过大,且甲苯对人体伤害较大。卡氏法能够较好地测定氨磷汀三水化合物的水分。结论：卡氏法测定氨磷汀三水化合物的水分需要样品量小、检测时间短、操作简便。     

抗生素药品干燥失重与费休氏水分测定方法比较

目的:通过比较试验考察两种水分测定方法有无显著性差异。方法:应用常压干燥失重法及费休氏法进行水分测定。结果:通过试验比较,干燥失重水分测定法与费休氏水分测定法无显著性差异。结论:部分药品的水分测定可用干燥失重法代替药典规定的费休氏法。     

PEG6000为载体的熊果酸固体分散体水分测定的研究

目的采用干燥失重法建立以PEG6000为载体辅料制备的熊果酸固体分散体的水分测定方法。方法先将样品在较低的温度（52℃）下干燥至大部分水分除去后,然后逐渐升温至105℃干燥至恒重。另应用甲苯法测定样品的水分。结果在低温（52℃）下可以将70%以上的大部分水分除去,在105℃极易恒重。测定结果同甲苯法无显著性差异。结论干燥失重法不需要特殊设备,简单易行、重复性好,可用于该制剂水分的测定。     

比较真空微波干燥法和热风循环干燥法对脉康宁胶囊流浸膏干燥后质量的影响

目的 比较真空微波干燥法和热风循环千燥法对脉康宁胶囊流浸膏干燥后质量的影响.方法 分别采用真空微波干燥法和热风循环千燥法对脉康宁胶囊流浸膏进行干燥,以性状、水分、浸膏得率、指标成分鉴别、含量测定和干燥效率为评价指标考察以上两种干燥工艺制得的干浸膏,比较不同干燥工艺的干燥效率和千燥后浸膏质量.结果 每干燥16 kg流浸膏...     

复方薄荷脑-硼酸氧化锌散的真空微波干燥工艺筛选

目的 筛选复方薄荷脑-硼酸氧化锌散的最佳真空微波干燥工艺.方法 采用L18(36)正交实验,以复方薄荷脑-硼酸氧化锌散的干燥失重、薄荷脑含量为量化考察指标,优选最佳干燥工艺.结果 优选的最佳真空微波干燥工艺为,干燥温度40℃,真空度0.7 MPa,干燥时间30 min,升温速度1℃/min,每盘物料平辅厚度约4 cm(...     

倍他米松磷酸钠标准改进及其对照品干燥失重方法修订的建议

目的:建立倍他米松磷酸钠标准中水分检测方法.方法:比较不同的干燥失重条件以及水分测定的结果,并通过动态水分吸附仪(DVS)对样品进行了考察.结果:采用水分测定法替代干燥失重检查可以避免干燥失重后样品降解.对照品使用前测定水分可以避免引湿性对对照品量值准确性的影响.结论:方法准确、方便,可作为倍他米松磷酸钠的水分检测方法.     

微波干燥在乌梅人丹生产中的应用研究

目的：比较乌梅人丹用烘箱干燥和微波干燥的效果。方法：以溶散时限、水分、薄荷脑含量、甘草酸含量为指标,比较其效果。结果与结论：微波干燥可提高产品质量、提高生产能力、降低能耗,优于烘箱干燥。。     

微波干燥与灭菌方法与传统方法效果比较

目的：研究微波干燥灭菌技术的特点和优点。方法：选用同种白一丸成品，运用微波和传统方法从时间、温度等方面考察干燥灭菌效果。结果：微波干燥灭菌方法效果明显优于传统方法。结论：微波干燥灭菌，不仅干燥速度快，能源利用率高，干燥灭菌效果好，成品质量高。     

Activity of antibiotic admixtures subjected to different freeze-thaw treatments

The freezing of antibiotic admixtures has been proposed as a potentially useful method by which the efficiency of admixture services might be improved. The time involved in thawing, however, has discouraged the implementation of this practice. This study describes a technique of thawing frozen antibiotic admixtures contained in minibags in commercially available microwave ovens. A quantitative microbiological agar gel diffusion assay was employed to determine the effect of such treatment on the antibiotic activity of the admixture. Admixtures containing cephalothin sodium, cefazolin sodium, cefamandole nafate, cefoxitin sodium, penicillin G potassium, ampicillin sodium, oxacillin sodium, carbenicillin disodium, and gentamicin sulfate in dextrose 5% solution were frozen at -20 degrees C for 30 days. The admixtures were assayed immediately before freezing, and again after either thawing technique: that is, upon exposure of the minibags to room temperature air or to microwave radiation. Assays were also performed 8 and 24 hours after thawing in order to assess antibiotic stability following each freeze-thaw treatment. It was discovered that, with the exception of ampicillin sodium, each of the antibiotics studied could be frozen and thawed as described without significant loss of activity, and were stable for 24 hours after thawing. The application of a freeze microwave-thaw technique to central admixture services can be seen as a cost-effective method of circumventing many of the problems associated with existing programs.     

In-line monitoring of granule moisture in fluidized-bed dryers using microwave resonance technology

This is the first report on in-line moisture measurement of pharmaceutical products by microwave resonance technology. In order to meet the FDA’s PAT approach, a microwave resonance sensor appropriate for pharmaceutical use was developed and implemented into two different fluidized-bed dryers. The novel sensor enables a continuous moisture measurement independent from the product density. Hence, for the first time precise real time determination of the moisture in pharmaceutical granules becomes possible. The qualification of the newly developed sensor was performed by drying placebo granules under experimental conditions and the validation using drug loaded granules under real process conditions. The results of the investigations show good correlations between water content of the granules determined by the microwave resonance sensor and both reference methods, loss on drying by infrared light exposure and Karl Fischer titration. Furthermore, a considerable time saving in the drying process was achieved through monitoring the residual water content continuously by microwave resonance technology instead of the formerly used discontinuous methods.     

微波技术干燥胃舒散的正交试验研究

目的:筛选微波技术干燥胃舒散的最佳工艺条件。方法:采用正交试验法,以干燥时间、微波功率、药粉粒度等因素为指标,考察胃舒散中水分的含量。结果:药粉粒度为24目筛的胃舒散以微波低火档(800W×58%)间断干燥6min(1.5min×4)为最佳干燥条件。结论:优选工艺干燥效果好、时间短。     

Physicochemical characterization of tacrolimus-loaded solid dispersion with sodium carboxylmethyl cellulose and sodium lauryl sulfate

To develop a novel tacrolimus-loaded solid dispersion with improved solubility, various solid dispersions were prepared with various ratios of water, sodium lauryl sulfate, citric acid and carboxylmethylcellulose-Na using spray drying technique. The physicochemical properties of solid dispersions were investigated using scanning electron microscopy, differential scanning calorimetery and powder X-ray diffraction. Furthermore, their solubility and dissolution were evaluated compared to drug powder. The solid dispersion at the tacrolimus/CMC-Na/sodium lauryl sulfate/citric acid ratio of 3/24/3/0.2 significantly improved the drug solubility and dissolution compared to powder. The scanning electron microscopy result suggested that carriers might be attached to the surface of drug in this solid dispersion. Unlike traditional solid dispersion systems, the crystal form of drug in this solid dispersion could not be converted to amorphous form, which was confirmed by the analysis of DSC and powder X-ray diffraction. Thus, the solid dispersion system with water, sodium lauryl sulfate, citric acid and CMC-Na should be a potential candidate for delivering a poorly water-soluble tacrolimus with enhanced solubility and no convertible crystalline.     

甲磺酸倍他司汀标准中存在问题和修改建议

目的:鉴于甲磺酸倍他司汀对热不稳定,并有引湿性,须修订水分检查方法。方法:分别考察HPLC,TLC和DSC纯度测定结果,及样品在不同相对湿度条件下的引湿性。结果:干燥失重对甲磺酸倍他司汀的纯度造成潜在影响,采用卡氏水分测定法替代70℃减压干燥24 h法。结论:《日本药局方》中干燥失重方法使甲磺酸倍他司汀纯度降低,新方法准确、方便,可作为甲磺酸倍他司汀的检查方法。     

注射用哌拉西林钠质量评价

目的:对不同生产工艺哌拉西林钠的质量进行对比研究及评价。方法:运用水分、水活度、酸度、有关物质等方法测定不同工艺产品,同时进行加速试验,并将测定结果进行多因素相关分析,综合评价不同工艺产品的质量。结果:冷冻干燥样品的水分、水活度、有关物质测定结果明显低于喷雾干燥样品,pH高于喷雾干燥样品,且产品的稳定性较喷雾干燥样品好。结果表明,水分与产品质量密切相关。结论:控制水分是保证本品质量的关键环节;应对现行标准部分项目控制指标予以修改;研究表明冷冻干燥工艺生产的原料质量较好,且不易受环境因素的影响,应当引导企业主动使用该原料。     

Evaluation of methods for the determination of water in substances with unknown chemical and thermal behaviour

The water content of six different substances was determined by means of five different methods. The methods used were loss on drying, thermogravimetry (coupled with DSC), a new phosphorous-pentoxide method, direct Karl-Fischer titration and the Karl-Fischer oven. A combination of direct Karl-Fischer titration and the KF-oven method was found to be the optimal technique for water determination of substances of unidentified chemical and thermal behaviour based on detailed considerations about selectivity, type of water binding, sample properties and efficiency.     

费休氏法测定罗红霉素颗粒水分

目的:建立费休氏法测定罗红霉素颗粒水分方法。方法:样品以无水甲醇为溶剂,采用无吡啶费休试液按中国药典方法测定。结果:测定结果与干燥失重法基本一致,平均回收率99.93%,RSD为0.31%。结论:该方法简便快速,定量准确,可作为罗红霉素颗粒水分测定方法。     

Dissolution and spectrophotometric determination of astaxanthin in aqueous solutions

The poor solubility of astaxanthin in water can cause problems during dissolution tests of dosage forms because they are usually performed in water-based media. The aim of this study was the development of a convenient dissolution medium and a method for a spectrophotometric determination of astaxanthin in an aqueous solution. Three surfactants in different concentrations were tested as solubility-improving substances: sodium lauryl sulfate (SLS), polysorbate 80 (PS 80) and macrogolglycerol hydroxystearate (Cremophor RH 40, CR 40). Optimal conditions were determined. The dissolution of astaxanthin from solid dosage form is performed into 1000 g of a solution of sodium lauryl sulfate with the concentration 1.0% (w/w) at 37 degrees C by paddle method, 100 rotations per minute, dissolution time 30 minutes. The procedure is convenient for solid dosage forms with a content of 4 to 12 mg of astaxanthin. The spectrophotometric determination of astaxanthin in aqueous solution from the dissolution test is measured at 486 nm. The specific absorbance A(1%) 1cm for astaxanthin in water is 2000, a sodium lauryl sulfate solution (1%) was used as a blank.     

他唑巴坦中结晶水的研究

目的考察国产他唑巴坦中是否结合有结晶水。方法采用卡尔费休氏水分测定法、干燥失重、热重分析法、热差分析法、单晶X-射线衍射的方法对他唑巴坦中的水分进行研究。结果用不同的常规水分测定方法对同一批他唑巴坦测定的结果有明显的差异。结论国产他唑巴坦1分子结合有0.5分子结晶水,结晶水与他唑巴坦分子结合紧密。