| In recent decades, with the rapid development of the global pharmaceutical industry, pharmaceutical intermediates industry have made much progress. A good trend and extensive application prospect both at home and abroad has been seen.3,3,3-Trifluoropropionic acid is a new-type pharmaceutical intermediate containing fluorine. Because of containing CF3special group, it has many unique excellent properties, and can synthetize a lot of important medicine, pesticide and polymer organic intermediates containing fluorine. Triphenylchloromethane is another kind of important pharmaceutical intermediates. It can be used for synthetizing antiviral and cephalosporin drugs, and also can be a kind raw material to synthetize triphenylmethanol and tritylnitrile. Besides, it can be used as hydroxyl and amino protective reagent.3,3,3-Trifluoropropionic acid and triphenylchloromethane are broad-spectrum and promising. Their demand are very large at home and abroad. At present, analytical research about3,3,3-trifluoropropionic acid and triphenylchloromethane is very rare. In order to develope and make use of them better, and provide guarantee for quality control, in this paper a study of analytical method on them, respectively, are developed by gas chromatography and high performance liquid chromatographic method combined with pre-column derivatization.The main content of this thesis are as follows:1. The first chapter of this thesis is a review related to some research about development and utilization of3,3,3-trifluoropropionic acid and triphenylchloromethane, pretreatment technology of derivatives and chromatographic analysis technique. Also the research content and purpose of the whole thesis were described in this chapter.2. In the second chapter, a new qualitative and quantitative method with gas chromatography and pre-column derivatization was developed for the determination of3,3,3-trifluoropropionic acid samples and its impurities. Sample pretreatment and chromatographic separation conditions were studied in this chapter. By comparing several derivative methods, we decided to use BF3-CH3OH as derivatization reagent treating3,3,3-trifluoropropionic acid sample finally. Then the derivative reaction conditions were optimized. The results showed that, when derivatization reagent was6%BF3-CH3OH, and its volume was3mL, reaction temperature was70℃, reaction time was60minutes, the reaction reacted completely.The derivation ratio can amount to99.8%. After separation conditions of gas chromatography were optimized, a gas analytical method for the determination of derivative products of3,3,3-trifluoropropionic acid sample was set up.Then the content of samples was detected by using butyl acetate as internal standard. Under those conditions, standard curve correlation coefficient of3,3,3-trifluoropropionic acid was0.9997.The relative standard deviation was0.05%. The recovery rates were between98.24%-101.49%.The detection limit of sample and its impurities were low. The method can be used for batch detection because of high sensitivity and good linearity. The accuracy and precision can meet analytical requirements. The research may provide practical value for the producers of3,3,3-trifluoropropionic acid. It can also be used as a analytical method of relative product content of3,3,3-trifluoropropionic acid3. In the third chapter, a new analytical method for the determination of triphenylchloromethane and its impurities was established by HPLC-UV detection and using methanol as a pre-column derivatization reagent. The conditions of derivative reaction and separation conditions of HPLC were optimized,respectively. With external standard method, the content of principal component and impurities in triphenylchloromethane samples was determined by the developed method. The best separation conditions of HPLC were the follows.UV detection wavelength was220nm. Mobile phase was acetonitrile-THF solution (acetonitrile/THF=95/5). Chromatographic column was Diamosil ODS-C18column. The column temperature was30℃. The flow rate was0.5mL/min. Under those conditions, standard curve correlation coefficient of triphenylchloro-methane was0.9997. The relative standard deviation was0.1%. The recovery rates were between98.04%-101.58%.The detection limit of sample and its impurities were low. The method had high sensitivity and good linearty. The results showed that accuracy and precision can meet analytical requirements.The developed method can be used for the the determination of triphenylchloromethane. The method has been applied to the determination of product batch. So it has certain practical value for the producers. |
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