1.Preparation of Electrochemical Sensor for Salicylic Acid Based on Molecular Imprinted Film
Chenggen XIE ; Huaifen LI ; Chunyan XIE ; Hankun ZHOU
Chinese Journal of Analytical Chemistry 2009;37(7):1045-1048
Molecular imprinted film modified glassy carbon electrode was prepared by electrochemical polymerization of pyrrole with the cyclic voltammetry in the presence of template molecular, salicylic acid. The template molecules were removed from the modified electrode surface by over-oxidized at 1.3V in the solution of 0.2 mol/L Na2HPO4 for 10 min. The modified electrodes can effectively promote electrochemical oxidation process of salicylic acid in the surface of electrode and avoid interference of structural similar substance such as benzoic acid. Cyclic voltammetry was employed in the electrochemical measurements. The experimental results show that the optimum acidity of background solution is pH 6.86 and the optimum incubation is 10 min. The linear response curve was obtained from 1.0×10-6 mol/L to 2.0×10-3 mol/L, with the detection limit of 8.0×10-7 mol/L. The imprinted electrode has been applied to the analysis of salicylic acid in the simulated samples with recovery rates ranging from 94.6% to 103.4%.
2.Determination of Organic Solvents Residue in Butoconazole Nitrate by Headspace Gas Chromatography
Weizhi LIU ; Hankun HU ; Ping LIU ; Wei LIU ; Mi ZHANG ; Baogen ZHENG ; Anni LIU ; Qiang YAN ; Lijuan ZHOU ; Yiming LIU
Herald of Medicine 2015;(8):1072-1074
Objective To establish a gas chromatograph method for determing Chloroform, ethyl acetate and N, N-dimethyl formamide in butoconazole nitrate. Methods The samples was detected by Headspace Gas Chromatography. Temperature programming method was adpoted and FID was used as detector. The injector temperature was 200 ℃, and the detector temperature was reach 250 ℃. Nitrogen was used as carrier gas in the experiment. Results In the mentioned chromatographic conditions, Chloroform, ethyl acetate and N, N-dimethyl formamide had good linear relationships in the ranges of 0. 066-0. 588,0. 062-0. 556 and 0. 896-8. 061 μg·mL-1 respectively. The average recoveries were 99. 18%,102. 84% and 98. 71%. RSD were 3. 87%,4. 33% and 3. 71%. Conclusion The detection method is sensitive, accurate, reliable, and can be used as a quality control for butoconazole nitrate.
3.Determination of Residual Organic Solvents in Fenticonazole Nitrate by Headspace Gas Chromatography
Weizhi LIU ; Hankun HU ; Wei LIU ; Mi ZHANG ; Baogen ZHENG ; Anni LIU ; Qiang YAN ; Lijuan ZHOU ; Yiming LIU
China Pharmacist 2015;(1):18-19,20
Objective:To establish a method for the determination of dichloromethane, methanol and ethanol in fenticonazole ni-trate. Methods:The samples were detected by headspace GC. The column was OV-1301(30 m × 0. 53 mm,3. 0 μm), the detector was FID with nitrogen as the carrier gas, the detector temperature was 250 ℃ and the injector temperature was 200 ℃. Results:The linear range of dichloromethane, methanol and ethanol was 2. 436-21. 924(r=0. 998 8), 12. 268-110. 412(r=0. 999 5) and 20. 052-180. 468 μg·ml-1(r=0. 996 9) with the average recovery of 99. 30% (RSD=2. 36%), 100. 21%(RSD=1. 07%) and 100. 15%(RSD=1. 21%)(n=9), respectively. Conclusion:The detection method is sensitive, accurate and reliable, and can be used in the quality control of fenticonazole nitrate.