高精度散射光度滴定法测定Al3+的含量

目的 探讨利用高精度散射光度滴定法测定AP3 含量的可行性。方法 用氢氧化钠的标准溶液作滴定剂，采用高精度散射光度滴定法对Al3 的含量进行测定，并将测定的结果与络合滴定法的测定结果相比较。结果 高精度散射光度滴定法的精密度可小于0．2％，经F检验表明与络合滴定法相当；t检验结果表明高精度散射光度滴定法的均值与络合滴定法无显著性差异。结论 高精度散射光度滴定法可以用于Al3 的含量测定。     

高精度散射光度滴定法测定盐酸异丙嗪的含量

目的　探讨高精度散射光度滴定法测定盐酸异丙嗪含量的可行性。方法　用四苯硼钠标准溶液滴定盐酸异丙嗪溶液 ,采用 0 .5 %聚乙烯吡咯烷酮溶液作为胶体保护剂。将测定结果与非水滴定法、电位滴定法和非水电位滴定法比较。结果　高精度散射光度滴定法含量测定结果的精密度小于 0 .2 %。F检验结果表明该方法精密度与药典方法相当 ;t检验结果表明方法的均值与药典方法无显著性差异。结论　所用方法可以用于盐酸异丙嗪的含量测定。     

高精度散射光度滴定法测定复方氯化钠注射液中氯化钾的含量

目的 研究复方氯化钠注射液中氯化钾的含量测定新方法。方法 用高精度散射光度滴定法代替四苯硼钠重量法。结果 高精度散射光度滴定法重复性好(RSD＝0．17％，n＝6)；准确度高，平均回收率为99．56％；与重量法所测定样品结果基本一致。结论 所用方法准确、便捷，适用于复方氯化钠注射液中氯化钾的含量测定。     

高精度散射光度滴定法在苯妥英钠含量测定中的应用

目的用高精度散射光度滴定法测定苯妥英钠。方法测定了苯妥英银凝胶的溶度积常数，研究了滴定的最优条件。结果滴定结果与对照试验测定结果无显著差异。结论用高精度散射光度滴定法测定苯妥英钠结果准确、重复性好、专属性强、线性范围宽。     

高精度散射光度滴定法测定盐酸环丙沙星的含量

采用高精度散射光度滴定法测定盐酸环丙沙星的含量,并与《中国药典》中的非水滴定法进行比较.含量测定结果的RSD ＜0.2％;F检验结果表明该方法的精密度与药典方法相当;t检验结果表明方法的均值与药典方法无显著性差异.     

高精度散射光度滴定法

目的建立高精度散射光度滴定法, 并将此方法应用于药物分析。方法利用内置散射光传感器检测滴定溶液中的散射光相对强度的峰值来判断滴定终点。以AgNO3溶液滴定NaCl溶液为例验证了高精度散射光度滴定法, 并以AgNO₃溶液滴定苯妥英钠溶液和NaOH溶液滴定盐酸普鲁卡因溶液为例验证了该方法在药物分析中的适用性。结果此法可适用于低浓度测定。在适当的条件下高精度散射光度滴定法的精密度和准确度均在0.2%以内。结论此法可应用于药物分析。     

络合法测定液体钙软胶囊钙含量

研究液体钙软胶囊钙含量的测定新方法,采用无消化的EDTA络合滴定法,测定结果与经典的原子吸收法无显著性差异.     

络合法测定液体钙软胶囊钙含量

研究液体钙软胶囊钙含量的测定新方法,采用无消化的EDTA络合滴定法,测定结果与经典的原子吸收法比较,差异无显著性。     

络合法测定液体钙软胶囊钙含量

研究液体钙软胶囊钙含量的测定新方法，采用无消化的EDTA络合滴定法，测定结果与经典的原子吸收法比较．差异无显著性。     

络合滴定法测定葡萄糖酸钙含量的不确定度评定

目的建立葡萄糖酸钙含量测定的不确定度评定方法。方法以评价络合滴定法测定葡萄糖酸钙含量的不确定度为例,分析滴定过程中不确定度分量的来源并进行评估〔2〕。结果扩展不确定度为0.25%,取κ=2（置信概率95）。结论通过分析不确定度的分量大小指导实验优化,使测定结果更加可靠。     

Highly accurate nephelometric titrimetry

A method that accurately indicates the end-point of precipitation reactions by the measurement of the relative intensity of the scattered light in the titrate is presented. A new nephelometric titrator with an internal nephelometric sensor has been devised. The work of the titrator including the sensor and change in the turbidity of the titrate and intensity of the scattered light are described. The accuracy of the nephelometric titrimetry is discussed theoretically. The titration of NaCl with AgNO(3) serves as a model. A relative error as well as deviation is within 0.2% under the experimental conditions. The applicability of the titrimetry in pharmaceutical analyses, for example, phenytoin sodium and procaine hydrochloride, is generally illustrated.     

Determination of norfloxacin by highly accurate nephelometric titration

A highly accurate nephelometric titration for the determination of norfloxacin is presented. The titration operating conditions were studied and the solubility product constant of norfloxacin-tetraphenylboron precipitation was determined. The result of the titration is comparable to those of control experiments. The proposed method has been found to be accurate, precise, specific, and linear.     

Determination of promethazine hydrochloride and its preparations by highly accurate nephelometric titration

A highly accurate nephelometric titration for the determination of promethazine hydrochloride and its preparations was presented. The titration operating conditions were studied and the solubility product constant of promethazine tetraphenylboron precipitation was determined. The result of the titration is comparable to those of control experiments. The proposed method has been found to be accurate, precise, specific and linear.     

Characterization of Opalescence in low Volume Monoclonal Antibody Solutions Enabled by Microscale Nephelometry

Monoclonal antibody (mAb)-based drugs are often prone to unfavorable solution behaviors including high viscosity, opalescence, phase separation, and aggregation at the high concentrations needed to enable patient-centric subcutaneous dosage forms. Given that these can have a detrimental impact on manufacturability, stability, and delivery, approaches to identifying, monitoring, and controlling these behaviors during drug development are critical. Opalescence presents a significant challenge due to its relationship to liquid-liquid phase separation. Quantitative characterization of opalescence via turbidimetry is often restrictive due to large volume requirements (>2 mL) and alternative microscale approaches based on light transmittance (Eckhardt et al., J Pharm Sci Technol. 1994, 48: 64–70) may pose challenging with respect to accuracy. To address the need for accurate and quantitative microscale opalescence measurements, we have evaluated the use of a ‘de-tuned’ static light scattering detector which requires <10 μL sample per measurement. We show that tuning of the laser power to a range far below that of traditional light scattering measurements results in a stable detector response that can be accurately calibrated to the nephelometric turbidity unit (NTU) scale using appropriate standards. The calibrated detector signal yields NTU values for mAbs and other protein solutions that are comparable to a commercial turbidimeter. We used this microscale approach to characterize the opalescence of 48 commercial mAb drug products and found that the majority have opalescence below 15 NTU. However, in products with mAb concentrations greater than 75 mg/mL, a broad range of opalescence was observed, in a few cases greater than 20 NTU. These measurements as well as nephelometric characterization of several IgG1 and IgG4 mAbs across a broad pH range highlight subclass-specific tendencies toward opalescence in high concentration solutions.     

Multiwavelength spectrophotometric determination of acid dissociation constants: Part III. Resolution of multi-protic ionization systems

A multiwavelength spectrophotometric (WApH) titration method was applied to study several multi-protic histamine H2-receptor antagonists which involved four acid dissociation constants (pKa values) over the pH range of 2-10. Specifically, UV absorption spectra of the drug solution were acquired in the course of a pH-metric titration using an optical device based on a fibre optics dip probe, a light source and a diode array detector. Target factor analysis was utilized to deduce the pKa values from the spectral data recorded at different pH. It was noted that some of the pKa values were within mid pH range which were difficult to obtain because of insufficient absorption spectra acquired in the un-buffered region of the titration curve. With the aid of the WApH technique coupled with an optically transparent buffer, all pKa values have been successfully determined and were in excellent agreement with those measured using a conventional pH-metric method.     

电位滴定法测定注射用青霉素钠含量

目的建立抗坏血酸自动电位滴定法测定注射青霉素钠含量的新方法。方法对仪器滴定参数、反应时间、反应温度、试剂用量、测定范围等影响因素以及反应的计量关系进行了考察。用0.01mol/L抗坏血酸标准溶液同步完成空白液Fe³⁺和反应液过剩Fe³⁺测定,计算青霉素钠含量。结果测定结果与设定浓度相对照,样品纯度在97.12%~99.86%之间,回收率控制在97.19~101.80%范围内,RSD<2.27%,最低检出量达到0.02mg。结论方法适合于注射使用青霉素钠纯度快速检测,也可用于课堂教学。