An efficient method is provided to detect simultaneously some important veterinary drugs from different classes in highly complex animal tissue matrix. This method using matrix solid-phase dispersion (MSPD) and high p...An efficient method is provided to detect simultaneously some important veterinary drugs from different classes in highly complex animal tissue matrix. This method using matrix solid-phase dispersion (MSPD) and high performance liquid chromatography (HPLC) with diode array detection (DAD) is developed to effectively determine two fiuoroquinolones (enoxacin and lomefioxacin), two sulfonamides (sulfanilamide and sulfamethoxazole) and one tetracycline (tetracycline) simultaneously in porcine tissues. In the process, MSPD methodology was used to treat samples, washed by n-hexane to remove lipid, eluted the analytes with acetonitrile–dichloromethane (1:1, v/v). Solvent acetonitrile and solvent acetic acid (0.1%) were combined in a gradient. HPLC–DAD analysis of the tissue samples was performed within 15 min at a fiow rate of 1.0 mL/min. The results showed that a recovery at 0.1, 0.5 and 1.0 mg/g fortification levels ranged from 80.6% to 99.2% with satisfactory relative standard deviations (RSDs) (below 6.1%, nfi3) and the limits of quantitation (LOQ) ranged from 7 mg/kg to 34 mg/kg in porcine tissues. Utilization of the method in successfully simultaneous analysis of porcine tissue incurred with veterinary drug multiresidues is described.展开更多
A gas chromatographic method without derivatization was developed for the residue analysis of 10 organonitrogen and 9 organophosphorus pesticides in soil and water. The samples were blended or shaken with acetone for ...A gas chromatographic method without derivatization was developed for the residue analysis of 10 organonitrogen and 9 organophosphorus pesticides in soil and water. The samples were blended or shaken with acetone for extraction. The extracts were cleaned up by coagulation, then, re-extracted with three 50 ml portions of dichloromethane. The final residue was detected by gas chromatography equipped with NPD. All of the 19 pesticides were completely separated at a constant temperature. The method described above was applicable to the simultaneous determination of 10 organonitrogen and 9 organophosphorus pesticides .in soil and water with the satisfactory recovery (from 82.42% to 103.57%), coefficient of variance (from 0.17% to 12.57%) and limit of detection (from 0.0006 ppm to 0.058 ppm).展开更多
A complete set of procedure for determination of multiresidue of pesticides in vegetables was presented in this paper.The complete set of procedure included three steps:bioassay,cholinesterase inhibition and GLC analy...A complete set of procedure for determination of multiresidue of pesticides in vegetables was presented in this paper.The complete set of procedure included three steps:bioassay,cholinesterase inhibition and GLC analysis.The samples could be identified to be contaminated with pesticides if 5% of house flies was knocked down in 50 tested house flies. Those samples contaminated with pesticides needed to be detected by AChE inhibition method.The qualitative and quantitative analyses were carried out by GLC.Recoveries ranged from 83.7% in Chinese cabbages to 105.6% in tomatoes for pyrethroids,and 84.0% in tomatoes to 102.7% in sweetbell redpeppes for organophosphorus compounds.Coefficients of variations ranged from 0.59% to organophosphorus compounds.Coefficients of variations ranged from 0.59% to 7.87% for pyrethroids. and 0.33% to 9.88% for organophosphorus compounds with vegetables. The complete set of procedure has been used successfully to analyze 7000 samples collected in Beijing. About 1% of the samples had a pesticide content exceeding the MRL.展开更多
A simplified method for determining 4 pyrethroid insecticides (Fenpropathrin, Cypermethrin, Fenvalirate, and Deltamethrin) in Chrysanthemi is described. Standards were fortified in to Chrysanthemi (5g) with two levels...A simplified method for determining 4 pyrethroid insecticides (Fenpropathrin, Cypermethrin, Fenvalirate, and Deltamethrin) in Chrysanthemi is described. Standards were fortified in to Chrysanthemi (5g) with two levels, 0.1-1 pp m the pyrethroid pesticides are extracted with petroleum ether and cleaned up by natural aluminum oxide. The extracts are analyzed by gas chromatography equipped with electron capture detector (ECD). Analysis of fortified Chrysanthemi (n = 3) shows recovery range from 99-102 % at 1 pp m level and 93-104 % at 0.1 pp m level. The coefficient of variation of the method at 1 st level was 0.12 and 0.14 for 2 ed level. The detection limits of the method ranged from 0.04pp b to 28 pp b. The method is rapid, sample, and sensitive and is applicable to the determination of Fenpropathrin, Cypermethrin, Fenvalirate, and Deltamethrin in Chrysanthemi.展开更多
基金supported by the Natural Science Foundation of Shaanxi Province (No. 2009jm4002-1)
文摘An efficient method is provided to detect simultaneously some important veterinary drugs from different classes in highly complex animal tissue matrix. This method using matrix solid-phase dispersion (MSPD) and high performance liquid chromatography (HPLC) with diode array detection (DAD) is developed to effectively determine two fiuoroquinolones (enoxacin and lomefioxacin), two sulfonamides (sulfanilamide and sulfamethoxazole) and one tetracycline (tetracycline) simultaneously in porcine tissues. In the process, MSPD methodology was used to treat samples, washed by n-hexane to remove lipid, eluted the analytes with acetonitrile–dichloromethane (1:1, v/v). Solvent acetonitrile and solvent acetic acid (0.1%) were combined in a gradient. HPLC–DAD analysis of the tissue samples was performed within 15 min at a fiow rate of 1.0 mL/min. The results showed that a recovery at 0.1, 0.5 and 1.0 mg/g fortification levels ranged from 80.6% to 99.2% with satisfactory relative standard deviations (RSDs) (below 6.1%, nfi3) and the limits of quantitation (LOQ) ranged from 7 mg/kg to 34 mg/kg in porcine tissues. Utilization of the method in successfully simultaneous analysis of porcine tissue incurred with veterinary drug multiresidues is described.
文摘A gas chromatographic method without derivatization was developed for the residue analysis of 10 organonitrogen and 9 organophosphorus pesticides in soil and water. The samples were blended or shaken with acetone for extraction. The extracts were cleaned up by coagulation, then, re-extracted with three 50 ml portions of dichloromethane. The final residue was detected by gas chromatography equipped with NPD. All of the 19 pesticides were completely separated at a constant temperature. The method described above was applicable to the simultaneous determination of 10 organonitrogen and 9 organophosphorus pesticides .in soil and water with the satisfactory recovery (from 82.42% to 103.57%), coefficient of variance (from 0.17% to 12.57%) and limit of detection (from 0.0006 ppm to 0.058 ppm).
文摘A complete set of procedure for determination of multiresidue of pesticides in vegetables was presented in this paper.The complete set of procedure included three steps:bioassay,cholinesterase inhibition and GLC analysis.The samples could be identified to be contaminated with pesticides if 5% of house flies was knocked down in 50 tested house flies. Those samples contaminated with pesticides needed to be detected by AChE inhibition method.The qualitative and quantitative analyses were carried out by GLC.Recoveries ranged from 83.7% in Chinese cabbages to 105.6% in tomatoes for pyrethroids,and 84.0% in tomatoes to 102.7% in sweetbell redpeppes for organophosphorus compounds.Coefficients of variations ranged from 0.59% to organophosphorus compounds.Coefficients of variations ranged from 0.59% to 7.87% for pyrethroids. and 0.33% to 9.88% for organophosphorus compounds with vegetables. The complete set of procedure has been used successfully to analyze 7000 samples collected in Beijing. About 1% of the samples had a pesticide content exceeding the MRL.
文摘A simplified method for determining 4 pyrethroid insecticides (Fenpropathrin, Cypermethrin, Fenvalirate, and Deltamethrin) in Chrysanthemi is described. Standards were fortified in to Chrysanthemi (5g) with two levels, 0.1-1 pp m the pyrethroid pesticides are extracted with petroleum ether and cleaned up by natural aluminum oxide. The extracts are analyzed by gas chromatography equipped with electron capture detector (ECD). Analysis of fortified Chrysanthemi (n = 3) shows recovery range from 99-102 % at 1 pp m level and 93-104 % at 0.1 pp m level. The coefficient of variation of the method at 1 st level was 0.12 and 0.14 for 2 ed level. The detection limits of the method ranged from 0.04pp b to 28 pp b. The method is rapid, sample, and sensitive and is applicable to the determination of Fenpropathrin, Cypermethrin, Fenvalirate, and Deltamethrin in Chrysanthemi.
