| Compared with the traditional separation methods, Capillary electrophoresis(CE) has many remarkable advantages such as fast separation, high efficiency and low consumption of samples. These peculiarities make CE rapidly develop into a very effective separation technology, which is widely used for the isolation of a broad range of compounds. Electrochemiluminescence (ECL), also known as electro-generated chemiluminescence, is an analytical technology combined with electrochemical method on the basis of chemiluminescence method. It has the advantages of high sensitivity, wide dynamic linear range and simplicity of chemiluminescence method. At the same time, it exhibits controllable property and good selectivity of electrochemical method. Thus, a new technology is formed by coupling capillary electrophoresis with electrochemiluminescence detection technique (CE-ECL). It offers the merits of CE with fast and efficient separation, less sample consuming, and also has the advantage of ECL with high selectiveness and sensitivity. By owing those advantages, CE-ECL detection is widely used in various fields like pharmaceutical analysis and bio-analysis, and also plays an important role in the separation and analysis of actual samples.Matrix solid phase dispersion (MSPD), introduced firstly by Barker in1989, is a sample treatment procedure used for the sample preparation, extraction and separation, and suitable for solid, semi-solid and biological samples of high viscosity. MSPD does not need of the homogenate, precipitation, centrifugal operation, and also avoids sample loss. Additionally, the method has many advantages such as efficiency, rapid separation and one step extraction, and conforms with environmental-friendly and economic requirements in modern society.This thesis is focused on the application of CE-ECL detection coupled with MSPD pretreatment method in pharmaceutical residue analysis. Its main contents were introduced as followings: 1. A novel, sensitive and rapid method for the determination of oxytetracycline residue in honey has been established using CE-ECL, based on the enhancement of oxytetracycline effecting on the Tris(2,2’-bipyridyl)ruthenium(Ⅱ). The effects of the detection potential, the pH and concentration of buffer, separation voltage, injection voltage and time on separation were investigated. Under optimal experimental conditions, the ECL intensity showed a good linear relationship (R=0.9950) in the linear range was20μg mL-1～200μg mL-1, the detection limit was5μg mL-1L-1. The method was successfully applied to the determination of oxytetracycline in the honey, and the recoveries were85.3%and81.6%, respectively.2. A CE-ECL method combined with MSPD pretreatment technology has been applied to the determination of pretilachlor. The effects of the detection potential, the pH and concentration of buffer, separation voltage, injection voltage and time and MSPD procedure were investigated. Under optimal experimental conditions, the ECL intensity showed a good linear relationship(R=0.9969) in the linear range from1×10-5tol*10-7mol L-1and. The detection limit (S/N=3) was6x10-8mol L-1and the recoveries was92.3-93.0%for rice and88.7-95.5%for soil.3. Clenbuterol hydrochloride, procaterol hydrochloride, salbutamol, terbutaline existing in pig fodder and pig urine were analyzed Using CE-ECL detection combined with MSPD.The effects of the detection potential, the pH and concentration of buffer, separation voltage, injection voltage and time on separation were investigated. Under optimal experimental conditions, the detection limit of these four β2-agonists drugs were0.081μmol L-1,0.076μmol L-1,0.074μmol L-1,0.12μmol L-1(S/N=3). The method was successfully applied to the analysis of β2-agonists drugs in pig feed and urine, and the recoveries were77.52%～102.51%and64.50%～110.67%respectively. |
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