A novel method for the determination of five carbamate pesticides (metolcarb, carbofuran, carbaryl, isoprocard and diethofencard) in water samples was developed by dispersive liquid-liquid microextraction (DLLME) ...A novel method for the determination of five carbamate pesticides (metolcarb, carbofuran, carbaryl, isoprocard and diethofencard) in water samples was developed by dispersive liquid-liquid microextraction (DLLME) coupled with high performance liquid chromatography-diode array detector (HPLC-DAD). Some experimental parameters that influence the extraction efficiency were studied and optimized to obtain the best extraction results. Under the optimum conditions for the method, the calibration curve was linear in the concentration range from 5 to 1000 ng mL^-1 for all the five carbamate pesticides, with the correlation coefficients (r^2) varying from 0.9984 to 0.9994. Good enrichment factors were achieved ranging from 80 to 177- fold, depending on the compound. The limits of detection (LODs) (S/N = 3) were ranged from 0.1 to 0.5 ng mL^-1. The method has been successfully applied to the analysis of the pesticide residues in environmental water samples.展开更多
Objective To establish a reverse-phase liquid chromatography method for the determination of seven alkaloids (magnoflorine, columbamine, jatrorrhizine, epiberberine, coptisine, palmatine, and berberine) in Fufang Zhen...Objective To establish a reverse-phase liquid chromatography method for the determination of seven alkaloids (magnoflorine, columbamine, jatrorrhizine, epiberberine, coptisine, palmatine, and berberine) in Fufang Zhenzhu Tiaozhi Capsule. Methods Chromatography was performed on a Dionex Acclaim C 18 column (250 mm × 4.6 mm, 5.0 μm) at 30 ℃ .The mobile phase was composed of acetonitrile-potassium dihydrogen phosphate solution (0.015 mol/L, 40:60, including 1.7 g/L sodium dodecyl sulfate and phosphoric acid used to regulate pH value to 3.0), with a flow rate of 1.0 mL/min. The detection wavelength was 270 nm. Results The calibration curves of magnoflorine, columbamine, jatrorrhizine, epiberberine, coptisine, palmatine, and berberine were linear in the range of 1.07- 10.65, 0.78-7.55, 0.75-7.50, 1.60-15.95, 2.69-26.85, 2.31-23.10, and 6.04-60.40 mg/mL. The average recoveries of magnoflorine, columbamine, jatrorrhizine, epiberberine, coptisine, palmatine, and berberine were 101.0%, 101.2%, 100.1%, 100.0%, 100.1%, 101.1%, and 99.7%, respectively. Conclusion The method could be used for the quantitative determination of the preparation.展开更多
基金supported both by the Natural Science Foundations of Hebei(No.B2008000210)the Scientific Research Foundation of Agricultural University of Hebei.
文摘A novel method for the determination of five carbamate pesticides (metolcarb, carbofuran, carbaryl, isoprocard and diethofencard) in water samples was developed by dispersive liquid-liquid microextraction (DLLME) coupled with high performance liquid chromatography-diode array detector (HPLC-DAD). Some experimental parameters that influence the extraction efficiency were studied and optimized to obtain the best extraction results. Under the optimum conditions for the method, the calibration curve was linear in the concentration range from 5 to 1000 ng mL^-1 for all the five carbamate pesticides, with the correlation coefficients (r^2) varying from 0.9984 to 0.9994. Good enrichment factors were achieved ranging from 80 to 177- fold, depending on the compound. The limits of detection (LODs) (S/N = 3) were ranged from 0.1 to 0.5 ng mL^-1. The method has been successfully applied to the analysis of the pesticide residues in environmental water samples.
基金Cooperation Project in Industry, Education and Research of Guangdong Province and Ministry of Education of China (2009B090300349)a Cooperation Project of National Science Foundation of Guangdong Province (10351022401000000)
文摘Objective To establish a reverse-phase liquid chromatography method for the determination of seven alkaloids (magnoflorine, columbamine, jatrorrhizine, epiberberine, coptisine, palmatine, and berberine) in Fufang Zhenzhu Tiaozhi Capsule. Methods Chromatography was performed on a Dionex Acclaim C 18 column (250 mm × 4.6 mm, 5.0 μm) at 30 ℃ .The mobile phase was composed of acetonitrile-potassium dihydrogen phosphate solution (0.015 mol/L, 40:60, including 1.7 g/L sodium dodecyl sulfate and phosphoric acid used to regulate pH value to 3.0), with a flow rate of 1.0 mL/min. The detection wavelength was 270 nm. Results The calibration curves of magnoflorine, columbamine, jatrorrhizine, epiberberine, coptisine, palmatine, and berberine were linear in the range of 1.07- 10.65, 0.78-7.55, 0.75-7.50, 1.60-15.95, 2.69-26.85, 2.31-23.10, and 6.04-60.40 mg/mL. The average recoveries of magnoflorine, columbamine, jatrorrhizine, epiberberine, coptisine, palmatine, and berberine were 101.0%, 101.2%, 100.1%, 100.0%, 100.1%, 101.1%, and 99.7%, respectively. Conclusion The method could be used for the quantitative determination of the preparation.