10384 985007 UDC 001.8 001.8 001 8
.. Abstract... 1 1.1.1 1...1 1.3.. 1.4..3.6.1.6..7..1...7.....8..3...8..4...10..5.11.3...1.3.1.1.3..13.3.3.13.3.4..17.3.5.19.4...0.5...6 9 3.1...9 3....30 3..1.31 3...31 3.3.3 3.3.1.3
3.3..35 3.3.3.36 3.3.4.37 3.4.39 3.4.1 MIP.39 3.4. MIP (SPE) 43 3.4.3 MIP.43 3.4.4 44 3.4.5 MIP.45 3.5...45.48 4.1...48 4. [NMIP ] 49 4..1 NMIP...49 4.. NMIP 50 4...1.50 4....50 4...3.51 4...4..54 4..3 NMIP..56 4.3 [EMIP] 60 4.3.1 EMIP 60 4.3. E(MIP) 60 4.3..1.60 4.3...61 4.3..3.63 4.3.3....64 4.4...67..7.. 73
I 1.. 3. 4. on-line in-situ 0.5~4.00g/mL,.0%45ng/mL 0.5~5.0g/mL,.%17ng/mL
1h 50g/g II
Abstract Abstract This dissertation consists of four parts:1.photochemical fluorimetry,. Photochemical fluorimetric characters of nitrazepam and estazolam,3.literature summary of molecular imprinted polymer(mip),4. Studies on preparation and characters of nitrazepam and estazolam imprinted polymer. In the first part, the dissertation summarized the principle and characters of photochemical fluorimetry,introduced the experimental techniques, including three fundamental types: on-line, in-situ and predetermined photochemical reaction. Except the above, the article summarized the application of photochemical fluorimetry. In the second part, a new method was developed for determination of nitrazepam and estazolam by photochemical fluorescence analysis (PCFA).This method has been applied to the determination of nitrazepam and estazolam in tablets, which obtained better results.photochemical reaction of nitrazepam and estazolam can occur under the irradiation of UV-light and produce a fluorescent product.the fluorescence intensity is linearly increased with the concentration of nitrazepam and estazolam.as to nitrazepam,the linear range lies between 0.5 and 4.00g/mL.The relative standard deviation and detection limit are.0% and 45ng/mL respectively. As to estazolam, the linear range lies between 0.5 and 5.0g/mL. The relative standard deviation and detection limit are.% and 17ng/mL respectively. The dissertation also do some research work about the mechanism of the photochemical reaction. In the third part, the dissertation summarized the origin, development and excellence of MIP in many fields, the principle of molecular imprinting technique(mit).a series of methods in the preparation of MIP were reviewed, including closed-tubes polymerization, in-situ polymerization, suspension polymerization and so on. The dissertation emphasized the applications of III
Abstract molecular imprinted technique in the fields of chromatography, SPE, sensors, artificial antibodies, catalysis. In the end, the dissertation also discussed the outlook of the technique. In the forth part, the molecular imprinted polymers with nitrazepam and estazolam were prepared at first, the absorption property and selective recognition ability were studied, the reasons of the absorption were discussed. During the course of polymerization, the template molecular, functional monomer, cross-linker and initiator were mixed under certain ratio, the mixtures were heated and polymerized. In the absorption experiment,the optimum absorption time is 1h,the maxi amount of binding was 50g/g for nitrazepam. In the selective experiment, we found that the MIPs have good selectivity. At last, we primarily studied the interaction between the functional monomers and the template moleculars with H-NMR.We found that this interaction is weak. As to the estazolam, the amount of absorption is smaller, which showed that the interactions between the functional monomers and the molecular polymers is very weak. How to choose proper polymerization entertainment and how to improve the reactions between moleculars still need to resolve. Keywords: Photochemical fluorimetry;nitrazepam ;Estazolam; Molecular Imprinted Polymers IV
Abstract V
1.1 Photochemical Fluorimetry, PCF 1947 Brodie [1] PCF 1. 1
/ [] 1.3 on-line in-situ 1.3.1 1-1 Tsushiya [3] HPLC PCF 00
PTFE 0.3-1.1mm, 0.5mm PTFE PTFE 300nm 30-400nm PCF [4~8] [7,8] [4~6] 1.3. PCF 1.3.3 PCF PCF PCF PCF TLC 1.4 3
Brodie [1] 1947 60 Goodyear [9] 70 HPLC [,7,8~15] TLC [,16] PCF PCF 1-1 1-1 F - NO - PO4 Mn + 3- Cr() Fe() 0.10ng/ml.0ng/ml 1.0ng/ml 0ng/ml 17 18 19 Clobazam.0ng/ml 4
5 Desmeyhyclobazam Zuclopenthixol Nedaltran Sulfaoyridine Deltamethrin Biacetyl K1 B1 B6 70pg 10pg 50pg 6.0~1ppb 1.0ng/ml 30pg 0.60ng/ml 1.0ng/ml 1.0ng/ml 1ng 30pg 40ng/ml 0.40ng/ml 0.30ng/ml 0.13ng/ml 0ng/ml 0.40ng/ml 0.60ng/ml 0.31ug/ml 0.016ng/ml 10ng/ml 0.66ng/ml 0.0ng/ml 1.710-8 mol/l 3.10-9 mol/l 0 1 3 4 5 5 6 7 8 9 30 31 3 33 34 35 57 58 59
.1 [36,37] [38,39] [40,41] [4~44] [45,46] [47,48] [49,50] [51~53] [54,55] [56] [8,3] H O 6
H O 0.5~4.00g/mL,.0 %45ng/mL 0.5~5.0g/mL,.%0.017g/mL...1 F4500 LZ1010 ph-06 30w 6m 0.5mm PTFE UV-7400 - Nicolet 740 FT-IR spectrometer 5.0mg 40mL 50mL 100µg/mL 5.0µg/mL 0.1molL -1 NaOH 0.05 moll -1 ph ph 37.0%40.0%.. 7
10mL.0mL 1.0 ml 10mL PTFE 7min 0min ex=353nm em=460nm..3.1 353nm 460nm.1 a b 11 : : 8
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