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...     

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.     

A Spectrophotometric Method for the Determination of Buclizine Hydrochloride Using the Charge-Transfer Spectrum of Buclizine-Iodine Complex

Abstract

A simple and sensitive spectrophotometric method is described for the determination of buclizine hydrochloride in bulk and tablets form. The method is based on the formation of charge-transfer complex between buclizine, as n-donor, and iodine, as Δ acceptor, which measured spectrophotometrically at 295 and 355 nm. A Job's plot indicated a 1:1 complex between the drug and iodine and Beer's law was obeyed in a concentration range of 4–30 μg ml^?1. A more detailed investigation of the complex was made with respect to its association constant and the free energy change. The method is simple and sensitive and has been applied successfully to the analysis of laboratory-made tablets without any interference from the tablet excipients. To validate the method, the results obtained were compared statistically with a newly developed uv-derivative spectrophotometric method. The charge-transfer method was favored due to its higher sensitivity, cheap coast and available equipments.     

Binding Study of Phenformin with Bovine Serum Album Using a Combined Technique of Equilibrium Dialysis with Flow-Injection Chemiluminescence Detection

ABSTRACT

The interaction between phenformin hydrochloride and bovine serum albumin (BSA) was investigated by the methods of chemiluminescence combined with equilibrium dialysis technique. A novel N-bromosuccinimide (NBS)–eosin Y (EY) chemiluminescence (CL) method was established for the determination of phenformin. The mechanism of this chemiluminescence system was proposed. Optimization studies were performed to determine the phenformin. Under the optimal conditions, the CL intensity was linear for a phenformin concentration over the range of 4.6 × 10^?8 to 5.0 × 10^?5 g/mL. The detection limit was 1.5 × 10^?8 g/mL. The data obtained by the present equilibrium dialysis–CL system were analyzed using the Klotz plot and the Scatchard analysis. The results showed that the Klotz plot and the Scatchard plot are linear with good correlation coefficient, indicating that the phenformin has only one type of binding site on BSA. The binding parameters were the number of the binding sites n (1.02) and the estimated association constant K (2.66 × 10⁴ L/mol). The chemiluminescence system combined with equilibrium dialysis developed in this work demonstrated its use for determination of interaction between drug and protein by using relatively simple instrument.     

新型交联烯丙基葡聚精离子交换剂的合成和性能

本文以N，N’－甲叉双丙烯酰胺交联的烯丙基葡萄聚糖凝胶（CADB）为基体，分别合成了其羧甲基和二乙基氨基乙基两种衍生物，作为分离生物大分子的离子交换剂。研究了合成中诸因素的影响，并对其性能进行了测试。产品的全交换量分别为2．5～3．5mmol／g（CMCADB）和1．2～2．0mmol／g（DEAE－CADB）。     

Determination of antihypertensive mixtures by use of a chemometrics-assisted spectrophotometric method

A simple multivariate calibration method for analysis of two types of hypotensive mixture is described. The mixtures are composed of chlorthalidone with atenolol or chlorthalidone with both amiloride hydrochloride and atenolol. The components of the mixtures result in substantial spectral overlap—between 87.5 and 91.0%. Resolution of the mixtures under investigation has been accomplished mainly by using CLS and PCR methods. The components in each mixture have been simultaneously determined in three commercial dosage forms with high accuracy and without interference from commonly encountered excipients and additives. Good recoveries were obtained with both synthetic mixtures and commercial tablets. The results obtained were compared with those from pharmacopeial methods and found to be in good agreement. The results obtained from CLS and PCR were also compared with those obtained from a ¹D spectrophotometric method.     

Investigating the post-chemiluminescence behavior of phenothiazine medications in the luminol–potassium ferricyanide system: molecular imprinting–post-chemiluminescence method for the determination of chlorpromazine hydrochloride

A new post-chemiluminescence (PCL) phenomenon was observed when phenothiazine medications were injected into the reaction mixture after the chemiluminescence (CL) reaction of luminol and potassium ferricyanide had finished. A possible reaction mechanism was proposed based on studies of the kinetic characteristics of the CL, CL spectra, fluorescence spectra, and on other experiments. The feasibility of determining various phenothiazine medications by utilizing these PCL reactions was examined. A molecular imprinting–post-chemiluminescence (MI-PCL) method was established for the determination of chlorpromazine hydrochloride using a chlorpromazine hydrochloride-imprinted polymer (MIP) as the recognition material. The method displayed high selectivity and high sensitivity. The linear range of the method was 1.0×10⁻⁸∼1.0×10⁻⁶, with a linear correlation coefficient of 0.9985. The detection limit was 3×10⁻⁹ g/ml chlorpromazine hydrochloride, and the relative standard deviation for a 1.0×10⁻⁷ g/ml chlorpromazine hydrochloride solution was 4.0% (n=11). The method has been applied to the determination of chlorpromazine hydrochloride in urine and animal drinking water with satisfactory results.      

Simultaneous Analysis of a Ternary Mixture of Pharmaceuticals Containing Trimethoprim,Sulphamethoxazole, and Phenazopyridine Hydrochloride Using Third-Derivative and Zero-Order Photodiode Array Spectrophotometry

A simple and rapid method for the simultaneous analysis of a ternary mixture containing trimethoprim, sulphamethoxazole and phenazopyridine hydrochloride is reported. The procedure consists of extraction in 0.1 M hydrochloric acid, filteration and measurement of the amplitudes of the third-derivative spectra at 242 and 276 nm and the absorbance at 450 nm for the determination of trimethoprim, sulphamethoxazole and phenazopyridine hydrochloride, respectively. Good linearity, accuracy, precision and selectivity were found, and the method is proposed for routine quality control purposes, even for the uniformity of contents test.     

Influence on drug efficacy of the binding behavior of pioglitazone hydrochloride with tryptophan residues,and tyrosine residues in bovine transferrin

Abstract

The interaction of pioglitazone hydrochloride bound to tryptophan residues and tyrosine residues in bovine transferrin was investigated using synchronous fluorescence spectroscopy at various temperatures (298, 310, and 318?K). From binding constants and thermodynamic parameters, it was shown that 1:1 stable compound was formed by the electrostatic force interaction of pioglitazone hydrochloride bound to tryptophan residues and tyrosine residues in bovine transferrin. The extent of binding between pioglitazone hydrochloride and tryptophan residues in bovine transferrin was more than that between pioglitazone hydrochloride and tyrosine residues in bovine transferrin. At 310?K, the fluorescence quenching ratio number of tyrosine residues and tryptophan residues in bovine transferrin were 47.52% and 54.19%, respectively, which indicated that the fluorescence contribution of tryptophan residues was greater. At 310?K, pioglitazone hydrochloride-tyrosine residues(in bovine transferrin) binding rate were 55.60–73.82%, and the combined model was W?=??0.0315R²???0.1520R?+?0.7385. The value of Hill’s coefficients was greater than 1, which suggested that there was a positive cooperativity between pioglitazone hydrochloride and subsequent ligands. The results of molecular docking were consistent with that of experimental calculation.     

Study on the interaction of tropisetron hydrochloride and l-tryptophan by spectrofluorimetry and its analytical application

A new method to determine tropisetron hydrochloride with l-tryptophan in the medium with pH=9.0 was studied, which is based on the fluorescence quenching effect of tropisetron hydrochloride on l-tryptophan. The fluorescence quenching mechanism and various factors influencing fluorescence quenching were discussed. Under the optimum conditions, the linear range and detection limit were 0.03-12.0 and 0.01 μg/mL (correlation coefficient r=0.9970), respectively. The calibration curve equation was ΔF=6.17+12.56 C (μg/mL). RSD was 3.4% (c=4.0 μg/mL, n=5); the detection limit estimated (S/N=3) was 0.01 μg/mL. The proposed method had been successfully applied to determine tropisetron hydrochloride in real samples and the obtained results were in good agreement with the results of the official method.