湿法磷酸生产饲料级磷酸氢钙技术的探讨

对国内加硅浓缩深度脱氟法和石灰乳二段中和法，２种主要生产饲料级磷酸氢钙的方法进行技术探讨，针对我国磷矿资源富矿少、贫矿多的现状，建议采用石灰乳二段中和法生产饲料级磷酸氢钙。该法操作弹性大、原料适应性强、工艺流程短、设备简易、一次性投资少     

国内磷酸氢钙生产的现状及发展

介绍国内饲料磷酸氢钙生产的现状，目前国内外采用的生产方法。提出应加强对其工艺的研究开发，提高饲料磷酸氢钙的技术和管理水平     

复盐沉淀法脱除湿法磷酸中镁铝氟杂质的研究

研究复盐沉淀法脱除湿法磷酸中镁、铝、氟离子，介绍复盐沉淀法的基本原理、特点。该法可供磷酸浓缩前的净化，饲料磷酸氢钙和三聚磷酸钠生产过程中湿法磷酸的净化等生产流程中选择应用。     

磷酸氢钙生产过程中脱氟渣的利用

磷酸氢钙生产过程中脱氟渣的利用赵焕祥丁家龙（安徽省凤阳磷化工有限公司２３３１２２中图分类号Ｘ７８１１问题的提出我厂１９９５年新扩１万吨／年饲料级磷酸氢钙，由于狠抓产品质量和内部管理，产品供不应求。为适应市场，仍要扩大规模，但在生产过程中每年２万吨的脱...     

3万吨／年磷铵装置联产1万吨／年饲料级磷酸氢钙的可行性探讨

探讨料浆法磷铵装置联产饲料级磷酸氢钙技术的可行性，并详细分析了“联产”新工艺的技术及经济优势     

磷酸氢钙中氟化物检查方法改进

目的改进磷酸氢钙中氟化物的检查方法。方法采用银-氯化银电极为参比电极,氟离子选择电极法测定磷酸氢钙中氟化物的含量。结果氟离子浓度在10~1 000 ng.mL-1时,电位值差值(△mv)与氟离子浓度(ng.mL-1)的对数值呈良好线性关系。结论该法操作简便、结果准确可靠,重现性良好。     

咖啡因结晶工艺实验研究

<正> 一、工艺概述: 国内生产咖啡因的结晶工艺,一直采用结品槽静止结晶方法,该法成品结晶形大而完整,但需要大量结晶槽.设备利用率低,人工挖槽,体力劳动强度大。采用结晶罐在搅拌下结品.则能克服上述缺点.结晶离心可以实现机械化连续操作,     

赖氨酸磷酸氢钙片中磷酸氢钙的含量测定

目的 建立赖氨酸磷酸氢钙片中磷酸氢钙的含量测定方法。方法 采用原子吸收分光光度法,在422.7 nm波长处测定样品吸光度,采用标准曲线法计算磷酸氢钙的含量。结果 磷酸氢钙在25.88~77.63 µg·mL^-1浓度范围内,与吸光度值呈良好的线性关系A=0.005 8C+0.038 2 (r=0.999 05),加标平均回收率为99.39% (RSD=1.2%, n=9)。结论 该方法专属性强,准确度好,简单易行,可用于赖氨酸磷酸氢钙片中磷酸氢钙的含量测定。     

注射用葡萄糖离子交换树脂法生产工艺

目前我国生产注射用葡萄糖均采用口服葡萄糖结晶两次。若采用离子交换树脂法处理糖液,再经一次结晶,即可符合在注射用规格,不仅可提高收率,降低成本,还提高了产     

星点设计-效应面法优化五酯缓释片处方

目的:优化五酯缓释片的处方。方法:以羟丙甲基纤维素、磷酸氢钙的用量为考察因素,分别以3、8、14、22h取样时间点的体外累积释放度为考察指标,选用星点设计-效应面法优化处方,并对该结果进行验证。结果:优化的处方为羟丙甲基纤维素、磷酸氢钙的用量分别为13.30%～30.00%、14.14%～17.07%。结论:通过星点设计-效应面法建立的模型可用于五酯缓释片处方的优化,所建立的数学模型具有准确的预测性。     

唑来膦酸的合成

目的　以 2 - (咪唑 - 1-基 )乙酸盐酸盐为原料合成唑来膦酸。方法　采用反应物浓磷酸自身作为溶剂 ,以无水乙醇作为结晶溶剂 ,合成唑来膦酸。结果和结论　避免了有毒有机溶剂的使用 ,将产物收率由 4 1.0 %提高到了 5 8.8%。唑来膦酸的结构经1HNMR、MS得到确证。     

乙水杨胺-草酸共晶的制备、表征及溶解性研究

目的 以乙水杨胺为药物活性成分,草酸为共晶形成物,制备乙水杨胺-草酸共晶,研究乙酸杨胺-共晶在磷酸盐缓冲溶液(PBS)以及模拟胃液(SGF)中的溶解度。方法 采用溶液结晶法制备了由两分子乙水杨胺和一分子草酸组成的乙水杨胺-草酸共晶。将乙水杨胺和草酸加热溶于乙酸乙酯,缓慢降温至室温、析晶、抽滤干燥,即获得乙水杨胺-草酸共晶。应用单晶X射线衍射(SCXRD)、X射线粉末衍射(XRPD)、差示扫描量热法(DSC)对乙水杨胺-草酸共晶进行了结构表征,测试溶解度。结果 共晶在磷酸盐缓冲溶液以及模拟胃液中的溶解度分别为乙水杨胺的2.0倍和2.5倍。     

盐酸多西环素精制结晶工艺的改进

目的　考察多西环素精制结晶工艺条件。方法　用氯化氢 -乙醇代替CP盐酸进行精制结晶。结果　使用氯化氢 -乙醇代替CP盐酸可得到合格的盐酸多西环素结晶。结论　多西环素结晶时以氯化氢 -乙醇代替CP盐酸,质量易于控制,特别对产品的黑杂点控制有一定作用     

结晶法氨苄西林钠工艺研究

探讨导致溶媒结晶法制得氨苄西林钠澄清度变化的影响因素，经过实验对比发现氨苄西林钠中残留的异辛酸是导致原粉与胶塞接触后澄清度变化的主要因素。针对溶媒法氨苄西林钠澄清度问题，对各种生产工艺进行了分析，开发了ATN溶媒结晶新工艺，并对ATN溶媒结晶工艺各操作条件的变化对产品质量及收率的影响进行了系统研究，最后对ATN工艺进行了优化。     

基于GC-MS技术的金钱草干预结晶肾损伤小鼠血清代谢组学研究

目的 利用血清代谢组学方法监测结晶肾损伤相关的代谢变化,评价金钱草提取物治疗结晶肾损伤的作用。方法 将21只野生型C57BL/6小鼠随机分为3组：空白对照组、结晶肾损伤模型组和金钱草干预组。采用乙醛酸盐诱导小鼠结晶肾损伤模型,给予6 d相应的治疗后,取小鼠血清进行气相色谱-质谱联用仪分析,结合模式识别筛选模型组和对照组之间的差异代谢物,并以此评价金钱草的治疗作用。结果 血清代谢组学分析鉴定了14种结晶肾损伤相关的生物标志物,包括嘌呤代谢物、氨基酸代谢物、脂肪酸代谢物等,同时数据显示金钱草提取物对结晶肾损伤有改善作用。结论 金钱草提取物能够通过调节失衡的嘌呤代谢、氨基酸代谢、糖代谢等途径而发挥预防和治疗结晶肾损伤作用。     

山莨菪碱四个光学异构体的合成和分离

以6-(甲氧)亚甲氧基托品酮(Ⅰ)为原料,与(+)L-酒石酸或(-)D-酒石酸成盐,可分离得到右旋的6-(甲氧)亚甲氧基托品酮[(+)Ⅰ]和左旋的6-(甲氧)亚甲氧基托品酮[(-)Ⅰ].(+)Ⅰ和(-)Ⅰ氢化还原后,分别与α-甲酰基苯乙酸甲酯进行酯交换,硼氢化钠还原侧链上醛基,水解脱去羟基保护基得到左旋山良菪碱(-)Ⅳ和右旋山莨菪碱(+)Ⅳ.(-)Ⅳ和(+)Ⅳ分別与(-)二苯甲酰酒石酸和(+)二苯甲酰酒石酸成盐,可用分步结晶法拆分到山崀菪碱的四个光学异构体。     

Differences in Crystallization Behavior Between Quenched and Ground Amorphous Ursodeoxycholic Acid

Purpose. To study the crystallization of ground and quenched ursodeoxycholic acid (UDCA) and to characterize their amorphous states. Methods. Amorphous UDCA was prepared by grinding and also by rapid cooling of the melt. These samples were characterized by powder X-ray diffraction (XRD), near IR spectra and dynamic water sorption. The heat associated with crystallization was measured in an isothermal microcalorimeter at 25°C at various relative humidities (RH) (50%–100%) and, in the presence of the vapour from a mixed solvent of ethanol and water (ethanol conc. 10%–100%). The specific surface area was calculated from krypton adsorption. Contact angles were measured by using a Wilhelmy plate to calculate the surface energy of the samples. Results. Ground and quenched samples yielded amorphous XRD patterns. Differential scanning calorimetry thermographs of the milled sample revealed that crystallization occurred at around 80°C, whereas the quenched sample did not crystallize. Exposure to humid air did not result in crystallization of either amorphous sample during the microcalorimetric experiments. In the presence of ethanol vapour, the ground sample did, but the quenched sample did not, crystallize. The amount of water sorption into the quenched sample was larger than that of the ground sample at low RH. The surface energy of the quenched material was different to that of the ground. Peak shifts were observed in the NIR spectra at around 1450, 2100 nm, allowing differentiation between the ground and quenched samples. Conclusions. It can be concluded that different molecular states of amorphous UDCA were obtained depending on the preparation method. The crystallisation of amorphous UDCA was related to the molecular state of disorder.     

Sustained release spherical agglomerates of polymethacrylates containing mefenamic acid: in vitro release,micromeritic properties and histological studies

Mefenamic acid (MA) spherical agglomerates (SAs) were prepared with various polymethacrylates having different permeability characteristics (Eudragit RS 100, Eudragit RL 100 and Eudragit L 100) and also with combination of Eudragit RS 100 and Eudragit L 100 in different ratios. SAs were prepared by spherical crystallization method using ethanol/dichloromethane solvent (crystallization) system. The influence of various formulation factors on the encapsulation efficiency, as in vitro drug release, and micromeritic properties was investigated. Target release profile of MA was also drawn. The yields of preparation and the encapsulation efficiencies were high for all formulations. The shape and surface characteristics of SAs were observed by a scanning electron microscope. The particle sizes are in the range of 0.219?±?0.1 to 0.482?±?0.25?mm (mean ± confidence interval t_95%). In addition, histological studies showed that the administration of MA in SAs containing Eudragit RS/L provided a distinct tissue protection in the stomach and duodenum. Differential scanning calorimetry and X-ray diffraction of powder studies showed that MA particles crystallized in the presence of polymethacrylates did not undergo structural modifications.     

Foundations of chemical microscopy, 2 derivatives of primary phenylalkylamines with 5-nitrobarbituric acid

5-Nitrobarbituric acid (dilituric acid) was extensively used with great success as a chemical microscopic reagent for the qualitative identification of primary phenylalkylamines. This methodology was based on the characterization of observed crystal morphologies, since a unique crystal habit could be associated with each adduct product. To understand the scientific foundations which permitted chemical microscopy to function as a useful analytical technique, the products formed between dilituric acid and a series of primary phenylalkylamines were characterized using polarizing optical microscopy, powder X-ray diffraction, thermal analysis, and solid-state nuclear magnetic resonance. It was deduced that the origins of the different crystal morphologies associated with each of the crystalline adducts arose from the ability of the systems to form differing structural types and/or hydrates upon crystallization. The degree of hydration in the crystalline phenylalkylamine adducts appeared to increase as additional carbon atoms were added between the aromatic ring and the terminal amine group of the aliphatic sidechain.     

甘露醇-旋光法测定鞣柳硼三酸散中硼酸的含量

目的建立旋光法测定鞣柳硼三酸散中硼酸的含量。方法以低浓度明胶溶液提取制剂中硼酸,利用甘露醇结合硼酸形成具有旋光性复合物,并建立鞣柳硼三酸散中硼酸的含量测定方法。结果硼酸浓度在5～20 g.L-1的浓度范围内与旋光度线性关系良好(r=0.999 2),方法的平均回收率为99.98%,RSD为1.3%。结论旋光法测定鞣柳硼三酸散中硼酸的含量,操作简便、快速,结果准确,重现性好。