Development and validation of a multiresidue method for determination of 37 pesticides in soil using GC-NPD.

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.

Determination of acetamiprid residues in zucchini grown under greenhouse conditions: application to behavioral dynamics.

A simple analytical method was developed for the determination of acetamiprid residues in zucchini and zucchini leaves grown under greenhouse conditions using liquid chromatography. Residues were confirmed via tandem mass spectrometry in positive-ion electrospray ionization mode. The calibration curves were linear with correlation coefficients in excess of 0.999. The limits of detection and limits of quantification were 0.01 and 0.03 µg/g and 0.02 and 0.06 µg/g, for the zucchini and zucchini leaves, respectively. For validation purposes, recoveries studies were carried out at low and high levels, yielding recovery rates ranged from 85.7 to 92.2% in zucchini and from 90.5 to 101.9% in zucchini leaves, with a relative standard deviation of <12%. The results demonstrated that the pattern of acetamiprid dissipation followed pseudo first-order kinetics with a half-life of 1.9 and 2.5 days, respectively. The residues in zucchini leaves were substantially higher than in the zucchini plant itself. No residues were detected at 7 days post-application. The results of this study suggest that acetamiprid is acceptable for application in/on zucchini under the recommended dosage conditions.

Simultaneous multiresidue determination of 48 pesticides in Yeongsan and Sumjin River water using GC-NPD and confirmation via GC-MS.

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).