| Chemilumiescence (CL) is defined as the emission of radiation, usually in the visible or near infrared region, as a result of a chemical reaction. One of the reaction products is formed in an electronic excited state, and emits the radiation on falling to the ground state. CL analysis has been widely used in many fields such as pharmaceutical science, environmental science and life science due to its attracting features including high sensitivity, wide linear dynamic range, simple and inexpensive instruments and rapid analysis speed. However the relatively poor selectivity of the CL analysis itself greatly limits its direct application to the analysis of analyte in complicated samples. Great efforts were made to improve the selectivity of CL analysis mainly from two aspects: One is using some separation techniques, such as high performance liquid chromatography (HPLC) and capillary electrophoresis (CE). But these methods not only required relatively expensive and complicated instruments, but also be greatly limited by the unconformity of the separation conditions and CL reaction conditions.Molecularly imprinting technology (MIT) is a novel technology, which prepares the polymer that has special recognition and selectivity function for template molecule. Molecularly imprinted polymer (MIP) not only has excellent special recognition capacity compared with enzyme-substrate, antibody-antigen, receptor-ligand, but also has attractive features such as physical robustness, high strength, resistance to elevated temperature and pressure, and inertness towards acids, bases, metal ions and organicsolvents. Due to the high selectivity and stability of the MIP, MIP has been applied in several analytical fields such as pharmaceutical science, environmental science and food analysis and pesticide residues etc. Combined the MIP with solid phase extraction (SPE), CL selectivity and sensitivity would be greatly improved due to the special recognition capacity and preconcentration capacity of MIP respectively.The thesis is divided into two parts. Part one describes solid phase extraction in detail and reviews recent development and application in analytical chemistry during these recent years. Part two includes two aspects. The first aspect described the tudies of molecularly imprinted on-line solid-phase extraction combined with hemiluminescence for the determination of pazufloxacin mesilate and Chlortetracycline. The second ascept describes the determination of tobramycin with flow injection chemiluminescene1. Molecularly imprinted on-line solid-phase extraction combined with chemiluminescence for the determination of pazufloxacin mesilateA novel molecularly imprinted polymer solid-phase extraction (MISPE) with flow-injection chemiluminescence (FI-CL) for the determination of pazufloxacin mesilate (PZFX) was developed. The molecularly imprinted polymer (MIP) was synthesized by using PZFX as the imprinting molecule. A glass tube packed the particles of the MIP was employed as MISPE micro-column, which was connected into the sampling loop of the eight-way injection valve for on-line selective preconcentration and extraction of PZFX. The eluent of acetonitrile: acetic acid (9:1, v.v) was used as carrier for eluting the adsorbed PZFX to react with the mixture of cerium (Ⅳ) and sodium sulfite in the flow cell to produce strong CL.The relative intensity of CL was linear to PZFX concentration in the range from 2.5×10-9 to 2.5×1097 g mL-1. The limit detection was 7×10-10 g mL-1 (3σ) and the relative standard deviation for 5×10-8g mL-1 of PZFX solution was 3.7 % (n=7). This method has been successfully applied for the determination of PZFX in humane urine.2. Molecularly imprinted on-line solid-phase extraction combined with flow injection Chemiluminescence for the determination of ChlortetracyclineA novel molecularly imprinted polymer solid-phase extraction (MISPE) method combined with flow-injection chemiluminescence for determining chlortetracycline Hydrochloride has been developed. The MIP was synthesized by using tetracycline as the imprinting molecule which has the similar structure like chlortetracycline. A polytetrafluoroe-thylene(PTFE)tube packed particles of MIP was employed as MISPE micro-column and was connected into the sampling loop of the eight-way injection valve for preconcentration and extraction of chlortetracycline hydrochloride. The eluent was used as carrier for extracting the adsorbed chlortetracycline hydrochloride to react with cerium (Ⅳ) and rhodamine6G mixture in the flow cell to produce strong CL. Intensity of CL was linear with concentration of chlortetracycline hydrochloride from 2×10-8 g/mL to 1×10-6 g/mLand the limit detection is 4×10-9g/mL (3σ).This method has been successfully applied to the determination of chlortetracycline hydrochloride in liver of chicken sample. 3. The determination of tobramycin with flow injection chemiluminesceneA flow injection chemilumiluminescence method for the determination of tobramycin in serum is described. The method is based on that tobramycin can enhances the CL reaction of luminal with K7[Cu(IO6)2] in potassium hydroxide medium. The intensity of CL was linear to tobramycin concentration in the range from 6×10-8 to 2×10-6g/mL. The limit detection was 1.5×10-8g/mL(3σ) and the relative standard deviation for 5×10-7g/mL of tobramycin solution was 2.7%(n=7).The method has been successfully applied to the determination of tobramycin in serum. |
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