| In this article, the practical current situation and development of pharmaceutical analysis on common spectroscopy were summarized, especially AAS and UV-VIS. Because some drug molecules contain hetero-elements such as N, O or S, so these drμgs could be formed as complex with metal-ions. A series of new method for content analysis of drμg on spectrometry with metal-ions was established. The main research content was as follows:1. In the buffer solution of acetic acid and sodium acetate which pH was5.80, ibuprofen can react with Cu2+to form the complex which was insoluble in water. After extracted by ethyl acetate, the remainder Cu2+in the raffinate was determined by FAAS. It was found that the absorbance decreased with the increase of drμg concentration. Accordingly, a new method of indirect determination was established, which was simple and rapid for ibuprofen by Cu2+complexation extraction and FAAS. And a series of the optimized measurement condition were studied. The experiment results showed that there was a good linear relationship between△A, the absorbance difference among reagent blank and raffinate, and the concentration of ibuprofen in the range from20.6μg·mL-1to103μg·mL-1. The correient of the linear equation was0.9988, the determination limit of this method was15.3μg·mL-1, and the RSD was2.18%. It had been successfully used for the determination of ibuprofen samples, the recovery was between97.62%and101.2%, and the results were satisfactory.2. Naproxen was antipyretic analgesic non-steroidal anti-inflammatory drμg, it could form complex with Ni2+in a neutral medium. After extracted by ethyl acetate, the absorbance of remainder Ni2+in the inorganic phase was measured by FAAS. It was found that△A, the different absorbance between reagent blank and raffinate, had a good linear relationship with the quantity of naproxen. Therefore, a new method for indirect determination of naproxen by FAAS was established. Under the optimized conditions, the linear range of this method was between41.45μg·mL-1and331.59μg·mL-1, R2was0.9970, the detection limit was18.4jig·mL-1, and the RSD was1.06%. The method was applied to the determination of actual samples of different manufacturer, the results accorded with labelled amount, and the recovery was between95.95%and103.2%.3. Ampicillin was a semisynthetic penicillin, it could be degraded in alkaline condition. In the ammonia medium, the degradative products can form with Ni2+to the complex which mix proportion was2:1. The complex had a characteristic absorption peak at269nm, the maximum molar absorptivity was4.28×103L·mol-1·cm-1, stability constant was5.95×109. There was a good linear relationship between the absorbance of complex and the concentration of ampicillin. Accordingly, a new method of indirect determination of ampicillin based on Ni2+complexation and UV spectrophotometry was established. In the linear range from17.47μg-mL’1to69.88μg·mL-1, the regression equation was A=0.0124p氨苄西林+0.0053, R2was0.9990, the detection limit was0.52μg·mL-1, and the precision was0.61%. The method was applied to the actual sample test with the satisfactory results, the range of recovery was from98.68%to102.7%, and the SD was between0.7and1.7.4. In ammonia medium, carbocisteine can be formed with Cu2+to the stable complex which mix proportion was2:1, the stability constant was4.98×109. The complex had a characteristic absorption at237nm, and it prensented linear relationship between the absorbancy and the concentration of carbocisteine. Therefore, a new method for quantitative determination of carbocisteine by Cu2+complexation and UV spectrophotometry was established. In the best conditions, the linear range of this method was from17.9μg·mL-1to71.7μg·mL-1, correlation coefficient was0.9957, RSD was2.16%, and the detection limit was0.74μg·mL-1. The method was successfully applied to the quantitative analysis for the carbocisteine samples of different pharmaceutical factory. The result was accorded with the labeled amount, recovery was between96.84%and103.1%, and SD was between0.5and1.5.5. Thyroxine can react with Cu2+into a complex in alkalescent conditions, and the characteristic absorption of the complex was at270nm. It was found that the absorbance of the complex increased with the increase of the thyroxine concentration, so a new method for indirect determination of thyroxine by UV spectrophotometry was established. In the optimal condition, the linear range of the method was from77.69μg·mL-1to310.8μg·mL-1, R2was0.9976, detection limit was7.55μg·mL-1, and RSD was0.36%. It was applied to determine the content of commercial thyroxine tablet, the recovery was between97.83%and101.9%, and the SD was between0.6and1.4. Meanwhile, the reaction mechanism was discussed. The ratio between thyroxine and Cu2+was2:1in the complex, the stability constant of the complex was6.70×1011, and the molar absorption coefficient was1.29×103L·mol-1·cm-1. |
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