Several methods used for the multiresidue analysis of pesticides from the environment and drinking water have been reported. However, most of these reports dealt with a small number of targeted pesticides or some special groups. A method that is simple, faster, and more cost-effective than the environmental protection agency (EPA) method has been developed for the analysis of 82 frequently used pesticides in water samples obtained from Yeongsan and Sumjin rivers, as well as rice fields located in various locations around the two rivers. The samples were extracted by dichloromethane, and the pesticides were analyzed using a GC-electron capture detector (ECD), followed by confirmation with GC-MS. Recoveries were found to be between 82 and 120.1% for most of the tested pesticides, which were in agreement with the standard values dictated by the EPA. The method was potentially applied to 66 water samples for human consumption and 90 water samples from the rice fields and irrigation ditches that were collected from June to September 2007. Oxadiazon, butachlor, and alachlor were detected in some of the river water samples collected in June, iprobenfos (IBP) was detected in samples collected in August, and no pesticide was detected in September. On the other hand, chlorpyrifos-methyl, IBP, hexaconazole, diazinon, oxadiazon, butachlor, and isoprothiolane were detected at relatively high concentrations in 48 rice paddy field water samples collected between June and September 2007. Alachlor in one sample and procymidone in some of the rice paddy field water samples were also detected in trace amounts. The results were consistent with the temporal pattern of pesticide application in Korean rice fields.
A simple analytical method was developed for the determination of chlorfenapyr residues in leeks grown under greenhouse conditions. Residues were extracted by salting out, analyzed by gas chromatography with microelectron-capture detection, and confirmed via gas chromatography-mass spectrometry. The calibration curves were found to be linear with correlation coefficients (r(2) ) in excess of 0.998. The limits of detection and quantification were 0.0015 and 0.005 mg kg(-1) , respectively. For validation purposes, recovery studies were carried out at low and high levels. Yield recovery rates were 87.27-89.64% with a relative standard deviation <6%. A maximum of 0.32 mg kg(-1) of chlorfenapyr residue was detected in leek sample sprayed three times at 7 day intervals until 7 days prior to harvest. The results of this study suggest that chlorfenapyr is acceptable for application in/on leeks under the recommended dosage regimen.
In this study, a multiresidue analytical method for the detection of 37 pesticides in a soil matrix was developed and validated. The soil sample was fortified with a known quantity of pesticides at two different concentration levels (0.1 and 0.01 µg/g) and the analytes were extracted via a liquid-solid extraction method. The pesticides were separated on an HP5 capillary column and were analyzed with a gas chromatograph coupled to a nitrogen-phosphorous detector (GC-NPD). Method validation was accomplished with good linearity (r(2) = 0.994-0.999) within a considerable range of concentrations. Satisfactory recoveries (70.5-110.4%) were obtained with 32 pesticides at both spiking concentration levels, whereas five pesticides-dimepiperate, buprofezin, prometryn, pirimicarb, and fludioxonil-were recovered at relatively low levels (43.6-61.8%). The applicability of the method was demonstrated by analyzing field samples collected from 24 different sites around Yeongsan and Sumjin rivers in the Republic of Korea. No residues of the selected pesticides were detected in any of the samples. The developed method could be employed as a simple and cost-effective method for the routine detection and analysis of 37 pesticides in soil samples.
In this study, the residual levels of four insecticidal compounds (lambda-cyhalothrin, lufenuron, thiamethoxam, and clothianidin) were monitored in the pomegranate, in order to assess the risk to consumers posed by the presence of such residues. The insecticides were applied at the recommended dose rates onto pomegranate trees. The samples were then collected at harvesting time after several treatments (two, three, and four treatments). After sample preparation progressed through the clean-up procedure, lufenuron, thiamethoxam, and clothianidin residues were analyzed via a HPCL-UVD, and the lambda-cyhalothrin residue was analyzed via a GC-µECD. The versatility of this method was evidenced by its excellent linearity (>0.9998 to 1) at broad concentration ranges. The mean recoveries evaluated from the untreated sample spiked with two different fortification levels ranged from 72.45 to 113.90%, and the repeatability (as a relative standard deviation) resulted from triplicate recovery tests was in a range from 0.80 to 11.75%. The residues of all insecticides determined from treated pomegranate samples and their LOD levels (lunfenuron, 0.01; lambda-cyhalothrin, 0.005; thiamethoxam, 0.01; clothianidin, 0.02 mg/kg) were much lower than their MRLs (0.5 mg/kg).
In a continuation of our earlier work, a multiresidual analytical method using 48 frequently used neutral pesticides in a water matrix was developed and validated in this study. The samples were extracted with dichloromethane and the pesticides were analyzed via GC-NPD followed by confirmation with GC-MS. Good linearity was detected over a concentration range of 0.01-1.0 microg/mL with correlation coefficients (r(2) ) in excess of 0.982. The recoveries were measured between 70.7 and 111.4% for the majority of the targeted pesticides with relative standard deviations (RSDs) of less than 20%. The LODs and LOQs were in ranges of 0.1-2 and 0.33-6.6 microg/L, respectively. A total of 66 water samples were collected from different locations in Yeongsan and the Sumjin River, Republic of Korea, and were analyzed in accordance with the developed method. None of the water samples were determined to contain any of the targeted pesticides. The method has been shown to be simpler, faster, and more cost-effective than the method established by the Environmental Protection Agency (EPA).
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