共振散射光谱法测定药物制剂中盐酸氯丙嗪的含量

在弱酸性溶液中,盐酸氯丙嗪与十二烷基苯磺酸钠反应形成离子缔合物,导致体系的共振散射（RS）强度急剧增强,并产生新的共振散射光谱,最强散射波长为466nm。本文研究了体系的光谱特征、反应的适宜条件和共存物质的影响。在466nm处,盐酸氯丙嗪的浓度在0.266—12.8μg/mL范围内与体系的散射强度有良好的线性关系,检出限（3σ）为0.056μg/mL。据此,建立了一种测定盐酸氯丙嗪含量的简便、快速、高灵敏的共振散射新方法,且已用于盐酸氯丙嗪片剂和针剂中含量的测定,结果满意。     

Fe(Ⅲ)-5-Br-PADAP-CTMAB体系间接分光光度法测定盐酸羟胺

在 CTMAB存在下 ,基于盐酸羟胺能定量还原 Fe( )离子为 Fe( )离子 ,利用显色剂 5 - Br- PADAP建立了间接分光光度法测定盐酸羟胺的方法。在 p H3.6的 KHC8H4 O4 - HCl缓冲溶液中 ,Fe( ) - 5 - Br-PADAP络合物的最大吸收峰位于 75 0 nm处。盐酸羟胺含量在 0— 35 μg/ 2 5 m L范围内符合比耳定律 ,ε=2 .4 0× 10 4 L·mol-1·cm-1。本方法用于盐酸羟胺 (工业品 )的测定 ,结果令人满意。     

NMR法测定复方制剂3组份的相对含量

本文对复方制剂中盐酸伪麻黄碱（Pse)、盐酸苯海拉明（Dip)和氢溴酸右美沙酚（Dex)3组份进行了NMR相对含量的测定。RSD分别为2.22%、3．18％、3．35％，绝对误差（E）分别为1．87％、3．66％、4．23％，方法简便快速，且相当准确。     

Ullmann-type C–N coupling reaction catalyzed by CuI/metformin

A facile and efficient method for Ullmann-type C–N coupling reaction of amine and aryl halide catalyzed by CuI/metformin in EtOH is described. The advantages of this method are the use of an inexpensive and readily available catalyst and ligand, easy workup, shorter reaction time, improved yields, and the use of green solvent. Furthermore, this procedure is applied successfully for the modification of natural products, such as Vindoline and Tabersonin.     

A Sensitive Electrochemical Sensor for Moxifloxacin Hydrochloride Based on Nafion/Graphene Oxide/Zeolite Modified Carbon Paste Electrode

A carbon paste electrode (CPE) modified with Nafion, Graphene oxide and zeolite has been prepared and characterized, and the resulting Nafion/Graphene oxide/Zeolite modified carbon paste electrode (N/G/Z/MCPE) has been applied to the electrochemical detection of Moxifloxacin hydrochloride (MOXI). It exhibited a good electrocatalytic activity in phosphate buffer (optimum at pH 7.4), as pointed out by cyclic voltammetry (CV), and N/G/Z/MCPE can be exploited for MOXI detection by chronoamperometry, electrochemical impedance spectroscopy and differential pulse voltammetry. This latter was the most sensitive one and gave rise to a linear calibration curve in the 0.04 to 250 μM concentration range, with limits of detection and qualification estimated at 1.0 nM and 3.3 nM, respectively. Contrary to previous electrochemical sensors for MOXI (e. g., CPE modified with metal nanoparticles), this new sensor can be used for multiple successive analyses without needing to refresh its surface.     

Liquid chromatographic determination of sitagliptin either alone or in ternary mixture with metformin and sitagliptin degradation product

Two reversed-phase liquid chromatographic (RP-LC) methods have been developed for the determination of sitagliptin phosphate monohydrate (STG). The first method comprised the determination of STG alone in bulk and plasma; and in its pharmaceutical preparation. This method was based on isocratic elution of STG using a mobile phase consisting of potassium dihydrogen phosphate buffer pH (7.8)-acetonitrile (70:30, v/v) at a flow rate of 1 mL min⁻¹ with flourometric detection. The flourometric detector was operated at 267 nm for excitation and 575 nm for emission. In the second method, the simultaneous determination of STG and metformin (MET) in the presence of sitagliptin alkaline degradation product (SDP) has been developed. In this method, the ternary mixture of STG, MET and SDP was separated using a mobile phase consisting of potassium dihydrogen phosphate buffer pH (4.6)-acetonitrile-methanol (30:50:20, v/v/v) at a flow rate of 1 mL min⁻¹ with UV detection at 220 nm. Chromatographic separation in the two methods was achieved on a Symmetry^® Waters C18 column (150 mm × 4.6 mm, 5 μm). Linearity, accuracy and precision were found to be acceptable over the concentration ranges of 0.25-200 μg mL⁻¹ for STG with the first method and 5-160 μg mL⁻¹, 25-800 μg mL⁻¹ for STG and MET, respectively with the second method. The optimized methods were validated and proved to be specific, robust and accurate for the quality control of the cited drugs in pharmaceutical preparations.     

流动注射化学发光法测定盐酸溴己新

在碱性溶液中,N-溴代丁二酰亚胺可以氧化曙红Y产生化学发光,盐酸溴己新的存在可以显著地增强这一反应的发光信号.基于此,结合流动注射技术,优化了实验的条件,建立了测定盐酸溴己新的流动注射化学发光新方法.该方法测定盐酸溴己新的线性范围为7.0×10-6-3.0×10-4g/mL.检出限为3.2×10-6g/mL.对浓度为5...     

刚果红分光光度法测定盐酸环丙沙星

在pH 4.39的乙酸钠-盐酸缓冲溶液中,盐酸环丙沙星与刚果红发生离子缔合反应,其最大吸收波长位于500nm处,表观摩尔吸光系数ε=9.46×104L/（mol.cm）,盐酸环丙沙星浓度在0.8—3.2mg/L范围内呈良好的线性关系,线性回归方程为A=0.3635＋0.01113C（mg/L）,相关系数r=0.9966;检出限为9ng/L;RSD为1.6%,据此建立了测定盐酸环丙沙星的新方法。优化了对盐酸环丙沙星的测定条件。本法仪器设备简单,操作简便,体系稳定,回收率测定结果较满意。     

酶催化荧光光谱法测定盐酸多巴胺

利用盐酸多巴胺对血红蛋白酶催化荧光体系的猝灭作用,建立了酶催化荧光光谱法测定盐酸多巴胺的新方法.研究了该猝灭体系的最佳实验条件及动力学行为,测定的线性范围为2.1×10-8--8.4×10-4mol/L,检出限为8.2×10-9mol/L.对浓度为5.2×10-6mol/L的盐酸多巴胺进行11次平行测定,其相对标准偏差...     

显微拉曼光谱法研究盐酸丁咯地尔的热降解历程

本文采用显微激光拉曼光谱、红外光谱和热重技术等多种分析方法,对盐酸丁咯地尔的热降解机理进行了较为详细的研究。通过对原药及其热氧降解历程中间产物的拉曼光谱、红外光谱分析,证实了盐酸丁咯地尔的热氧降解过程与热重分析实验的结果基本相符。热降解过程分为两个明显的阶段:第一阶段是盐酸丁咯地尔脱盐酸、脱羧裂解,剩下苯环骨架结构;第二阶段是苯环骨架完全氧化裂解。