Study On The Novel Sample Preparation Methods For The Determination Of Chinese Medicinal Material And Preparation

In analytical chemistry, sample preparation is a pivotal process. Liquid-liquid extraction(LLE) is the classical method for sample preparation and preconcentration. Unfortunately, LLE is time-consuming, tedious, laborious and it requires large amount of toxic organic solvents, which have great threat on human health and environment. Therefore, simple, efficient, rapid and organic solvent-free sample preparation methods are required. Several pretreatment methods used in the analysis of Chinese Medicinal Material and Preparation were studied in this thesis. The thesis has 4 chapters and the main results are as follows:In chapter 1:Current existing pretreatment methods in pharmaceutical analysis were reviewed. Special emphasis was placed on the cloud point extraction, dispersed phase liquid-liquid microextraction and microwave assisted micellar extraction involving fundamental theory, experimental condition optimization and practical applications.In chapter 2:A new method for the determination of amikacin sulfate by cloud point extraction-UV/VIS spectrophotometry was established. The effects of pH, concentration of Triton X-100, cloud point temperature, time and interfering ions on the extraction efficiency were evaluated. The proposed method was applied to the determination of amikacin sulfate in amikacin sulfate injection and human urine with satisfactory results.In chapter 3:A novel dispersive liquid-liquid micro extraction (DLLME) coupled with high performance liquid chromatography method was developed for the determination of five anthraquinone derivatives. Some important parameters, such as the kind and volume of extraction solvent and dispersive solvent, extraction time and salt effect, were investigated and optimized. Under the optimum extraction condition, Aloe-emodin, Rhein, Emodin, Chrysophanol and Physcion in three oral solution of rhubarb were successfully analyzed.In chapter 4:A novel microwave assisted micellar extraction method coupled with high performance liquid chromatography was developed for the determination of five anthraquinone derivatives in semen cassiae. Some important parameters, such as the pH value of the solution, microwave assisted micellar extraction time, extraction power, the concentration of surface-active agent GenapolX-080 solution, liquid-solid ratio (mL/g), semen cassiae granularity, were investigated and optimized. Extraction efficiency was compared between microwave assisted extraction (MAE) and conventional extraction techniques, such as ultrasonic assisted extraction(UAE), extraction at room temperature(ERT). Higher extraction efficiency was obtained.