| An effective early diagnosis method for diabetes is a very important tool to prevent and treat diabetes. It has become one of the research focuses in the medical research field. In recent years, the early diagnosis of diabetes by detecting the metabolic markers in the body fluids of patients suspected is a potential way to improve the treatment of diabetes. However, there are a lot of interfering substances because of the complexity of the urine matrix, and the concentration of target molecule is relatively low. A highly selective sample preparation method for sample purification, separation, concentration combined with a rapid and sensitive detection method is desired for analysis of diabetic biomarker.Solid Phase Microextraction is a new sample preparation technique. The method is simple, fast, solvent-free and environmentally friendly. It combines sampling, isolation, enrichment in one step. This approach has been widely used in various fields.Dispersive liquid-liquid microextraction based on solidification of floating organic droplet method (DLLME-SFO) is developed recently. It was utilized only a small amount of solvent for concentrating analytes from samples. DLLME-SFO is a simple, fast and green sample preparation method. In this method, the low toxicity solvent which has lower density than water and the freezing point of the organic solvent near room temperature is selected as extraction solvent. After extraction, the low toxicity solvents rapidly condenses into a small ball in the liquid surface. This approach has also been widely used in various fields.In this work, two new sample preparation methods were developed for analysis of acetone in hunman body fluids by combination with HPLC. It provides a promising tool for non-invasive early diagnosis of diabetes. The main contents of study are as follows:1.Based on the poly(methacrylic acid-co-ethylene glycol dimethacrylate, MAA-co-EDMA), a novel ultrasound-assisted headspace solid-phase microextraction method was developed for the analysis of acetone in diabetic urine by combination with HPLC. We optimized the factors affecting the derivatization-extraction efficiency. The limit of detection value (LOD) based on the signal to noise ratio of3:1(S/N=3) was1.0nmol L-1for acetone The good linearity by this method was observed over the concentrations range of0.05to25μmol L-1. The present study provides a simple, rapid and sensitive approach for quantification of acetone in complex biological samples.2.A simple and rapid solid phase microextraction method coupling to HPLC was developed for the analysis of acetone in human urine samples.In this work, florisil was selected as solid sorbent of SPME. After derivatization, the analyte in solution was adsorbed by extract materials. A series derivatization reaction and extraction conditions were optimized in the experiment. The limit of detection value (S/N=3) is35.6nmol L-1, The intra-day and inter-day RSDs were less8.9%. The results show that the present method is sensitive and facilitates the early detection of disease markers in biological samples.3. A new dispersive liquid-liquid microextraction method based on solidification of floating organic droplet (DLLME-SFO) was developed for the determination of human urine samples.1-dodecanol was choose as the extractant. A series derivatization reaction and extraction conditions were optimized in the experiment. The limit of detection value (S/N=3) is2.9nmol L-1, the value for recovery of acetone was105.8%at low concentration level (0.25μmol L-1), and it was89.3%at high level (2.5μmol L-1). The concentrationt of acetone in urine samples of diabetic and healthy people was determined. The results show that the method has certain application value in the early diagnosis of diabetes. |
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