In this study, a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was established for the extraction and cleanup of fipronil and its three metabolites (fipronil solfone, sulfide, and desulfinyl) in peanut kernel, shell, straw, seedling, and soil samples, and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was used for analysis. The average recoveries were 66-116% at the level of 0.001-0.1 mg/kg with the RSD <19%, and the limit of detection was 0.3 ng/g for all matrices. The dissipation experiment results demonstrated that fipronil dissipated more rapidly in peanut seedling than in soil, with half-lives of <1 day in peanut seedling and 32-57 days in soil depending on the soil pH. The final residues at harvest of peanut kernels were all below 0.02 mg/kg, whereas in peanut shell and straw, the total highest residues were 0.99 and 0.30 mg/kg, respectively. Fipronil-desulfinyl and fipronil-sulfone were the highest residue metabolites in peanut plant (seedling and straw) and soil samples, respectively.

The dissipation and final residues of picoxystrobin in peanut and soil were determined by a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). The dissipation and final residue of picoxystrobin at three different provinces (Hebei, Hubei, and Shandong) in China were studied. The fortification experiments at three different spiking levels of 0.01, 0.05, and 0.5 mg kg(-1) in all matrices (soil, peanut seedling, shell, stalk, and kernels) were conducted, and the recoveries were 79-114% with relative standard deviations of 3-12 (n = 5). The dissipation half-lives of picoxystrobin were 1.5-8.6 days in soil, and 2.1-2.8 days in seedlings. The final residues of picoxystrobin in supervised field trials were 0.05-6.82 mg kg(-1) in stalk, ≤0.381 mg kg(-1) in soil, ≤0.069 mg kg(-1) in shells, and ≤0.005 mg kg(-1) in peanut kernels. Considering the final residue levels and the maximum residue limits (MRLs), the pre-harvest interval of 14 days was recommended for the safe use of picoxystrobin in peanut crop.

A multiresidue analytical method using a modification of the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) sample preparation approach combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis was established and validated for the rapid determination of 69 pesticides at different levels (1-100 ng/g) in wheat and rice straws. In the quantitative analysis, the recoveries ranged from 70 to 120%, and consistent RSDs ≤ 20% were achieved for most of the target analytes (53 pesticides in wheat straw and 58 in rice straw). Almost all of the analytes achieved good linearity with R(2) > 0.98, and the limit of validation levels (LVLs) for diverse pesticides ranged from 1 to 10 ng/g. Different extraction and cleanup conditions were evaluated in both types of straw, leading to different options. The use of 0.1% formic acid or not in extraction with acetonitrile yielded similar final outcomes, but led to the use of a different sorbent in dispersive solid-phase extraction. Both options are efficient and useful for the multiresidue analysis of targeted pesticides in wheat and rice straw samples.

A sensitive and rapid analytical method based on QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation and LC-MS/MS detection was developed for the analysis of halosulfuron-methyl residues in wheat. The recoveries of halosulfuron-methyl in both the wheat plant and grain ranged from 87% to 119% and from 75% to 97%, respectively, with relative standard deviations (RSDs) of 3-9%. The limit of quantification (LOQ) was 0.005 mg kg(-1) for wheat plant and 0.001 mg kg(-1) for wheat grain. The half-life of halosulfuron-methyl in the wheat plant was 0.9-9.5 days. The terminal residue levels of halosulfuron-methyl in wheat grain were below 0.01 mg kg(-1) at harvest.

This work is the first report on the dissipation and final residue of cloransulam-methyl on soybean plant at field conditions. A fast, simple, and reliable residue analytical method for determination of cloransulam-methyl in soybean matrices and soil was developed based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation and liquid chromatography-tandem mass spectrometry (LC-MS/MS) detection. The average recoveries of cloransulam-methyl in soybean matrices and soil ranged from 80 to 105%, with RSDs between 3-11%. The limit of detection (LOD) was 0.001 mg kg(-1) for soybean grain, plant, and soil and was 0.005 mg kg(-1) for soybean straw. This method was then used to characterize dissipation of cloransulam-methyl in soybeans and soil from three locations in China for the first time. Cloransulam-methyl dissipated quickly in soybean plant with half-lives (T1/2) of 0.21-0.56 days. The dissipation dynamic in soil was characterized using both first-order kinetics model and two-compartment model, and the half-lives were similar, ranging from 0.44 to 5.53 days at three experimental sites in 2012 and 2013. The final residue data showed a very low level of cloransulam-methyl in soil (≤0.026 mg kg(-1)), soybean grain (≤0.001 mg kg(-1)), and straw (≤0.005 mg kg(-1)) samples at harvest time. With the faster and simple analytical method on soybean and soil, rapid dissipation of cloransulam-methyl was observed at three geospatial locations in China, and the terminal residue levels were negligible, so mammalian ingestion exposure is minimal.