A novel heterocyclic system — dihydro-2H-1,5,2,4-dioxadiazine. 2,4-Dimethyldihydro-2H-1,5,2,4-dioxadiazine hydrochloride: synthesis and NMR study

The first representative of a novel heterocyclic system, namely, 2,4-dimethyldihydro-2H-1,5,2,4-dioxadiazine hydrochloride, was synthesized.     

主成分回归一紫外光度法同时测定盐酸西替利嗪和苯甲酸钠

提出了一种用紫外光度法同时测定盐酸西替利嗪和苯甲酸钠的方法.在pH 4.56的B-R缓冲溶液中对盐酸西替利嗪和苯甲酸钠两组分混合溶液进行吸光度测定,所得的重叠光谱数据用主成分回归法(PCR)和偏最小二乘法(PLS)等化学计量学方法进行处理,结果表明主成分回归(PCR)的预报误差最小.对实际样品进行测定,回收率为88.8...     

Non-equilibrium determination of metoclopramide and tetracaine hydrochloride by sequential injection spectrophotometry

A new sequential injection spectrophotometric method was proposed for the determination of metoclopramide and tetracaine hydrochloride. The method was based on the detection of an unstable red intermediate compound resulting from the reaction of metoclopramide or tetracaine hydrochloride with potassium dichromate, in the presence of sodium oxalate, in sulfuric acid solution. The related reaction mechanisms of this new method have been studied. The experimental conditions were optimized for the stopped-flow and continuous-flow sequential injection models. For continuous flow, the linear range for determination of metoclopramide, the detection limit and the sampling frequency were 13-130 μg ml⁻¹, 9.4 μg ml⁻¹ and 40 samples per hour, respectively. For stopped flow, they were 3-42 μg ml⁻¹, 1.0 μg ml⁻¹ and 18 h⁻¹, respectively. Adopting the continuous-flow model for tetracaine hydrochloride, the linear range was 25-300 μg ml⁻¹, and the detection limit was 18.0 μg ml⁻¹ with sampling frequency of 40 h⁻¹. This method has been used to determine metoclopramide and tetracaine hydrochloride in pharmaceutical preparations, and the results are compared with those determined by the pharmacopoeia method. Statistical analysis reveals that there was no evidence of significant difference between the methods.     

卤代-D,L-苯丙氨酸盐酸盐的合成与表征

以乙酰氨基丙二酸酯和苄卤为原料,经缩合、碱性水解、脱羧和脱乙酰基,合成了一组卤代-D,L-苯丙氨酸盐酸盐,利片j核磁共振谱(1H NMR)和质谱(MS)表征了产物的结构,利用元素分析确定了其组成.     

多壁碳纳米管修饰电极检测盐酸氯丙嗪的研究

制备了多壁碳纳米管修饰玻碳电极,采用循环伏安法(CV)研究了盐酸氯丙嗪在修饰电极上的电化学特性,发展了一种新的检测盐酸氯丙嗪的电化学分析方法。在最佳实验条件下,用循环伏安法检测盐酸氯丙嗪,其响应电流与盐酸氯丙嗪的浓度在8.0×10-5~1.0×10-3mol/L范围内有很好的线性关系,线性方程为Ip(A)=0.0106c(mol/L)-8×10-8(R2=0.999,n=6),检出限为6.2×10-6mol/L(S/N=3)。方法可用于盐酸氯丙嗪片的测定。     

盐酸克伦特罗在乙炔黑电极上的电化学行为及其分析测定研究

研究了盐酸克伦特罗(CLB)在乙炔黑电极上的电化学行为,发现阴离子表面活性剂十二烷基苯磺酸钠(SDBS)能显著提高CLB的氧化峰电流并降低其氧化过电位。优化了实验参数,建立了一种直接测定CLB的新电分析方法,其线性范围为1.0×10-7~7.5×10-5mol/L,开路富集1 min后的检出限为2.5×10-8mol/L。平行10次测定1.0×10-5mol/L盐酸克伦特的RSD为3.1%。方法用于猪尿中盐酸克伦特罗含量的测定。     

Crystal Structure and Thermodynamic Study of Ephedrine Hydrochloride C10H16NOCI（s）

The crystal structure of ephedrine hydrochloride was determined by means of X-ray crystallography.The crystal system of the compound is monoclinic,and the space group is P21.Unit cell parameters are a=0.7308(6) nm,b=0.6124(5) nm,and c=1.2618(11) nm;α=90°,β=102°,and γ=90°;Z=2.Low-temperature heat capacities of the title compound were measured with an improved precision automated adiabatic calorimeter over a temperature range from 77 K to 396 K.A polynomial equation of the heat capacities as a function of temperature in the temperature region was fitted by the least-squares.Based on the fitted polynomial equation,the smoothed heat capacities and thermodynamic functions of the compound relative to the standard reference temperature 298.15 K were calculated and tabulated at the intervals of 5 K.     

Novel Potentiometric Sensors for Determination of Melatonin and Oxomemazine in Biological Samples and in Pharmaceutical Formulations

Simple, selective and accurate sensors were developed for the determination of melatonin and oxomemazine in biological samples (urine) and in pharmaceutical preparations. Potentiometric measurements were based on bismus tetraiodate‐drug ion‐pair as novel electroactive materials incorporating a plasticized PVC membrane with o‐nitrophenyl octyl ether or dioctyl phthalate. Each sensor was conditioned for at least two days in 0.1 M drug solution before use. It exhibited fast and stable Nernstian response for melatonin and oxomemazine over the concentration range of 1.0×10^?6–1.0×10^?2 M and 1.0×10^?5–1.0×10^?2 M, pH range of 3.0–6.5 and 3.5–6.0 for melatonin and oxomemazine sensors, respectively. Results with an average recovery not more than 101 % and a mean standard deviation less than 1.0 % of the nominal were obtained for the four sensors. The sensors showed reasonable selectivity towards investigated drugs in presence of many cations.     

An efficient synthesis of 3,4-dihydropyrimidin-2(1H)-ones catalyzed by thiamine hydrochloride in water under ultrasound irradiation

An environmentally benign aqueous Biginelli protocol for the synthesis of substituted 3,4-dihydropyrimidin-2(1H)-ones using thiamine hydrochloride as a catalyst has been achieved. These ultrasound-assisted reactions proceed efficiently in water in the absence of organic solvent. Utilization of ultrasound irradiation, simple reaction conditions, isolation, and purification makes this manipulation very interesting from an economic and environmental perspective.