[Determination of three new herbicide residues in soil, sediment and water by liquid chromatography-tandem mass spectrometry].

Herbicides play an important role in preventing and controlling weeds and harmful plants and are increasingly used in agriculture, forestry, landscaping, and other fields. However, the effective utilization rate of herbicides is only 20%-30%, and most herbicides enter the atmosphere, soil, sediment, and water environments through drift, leaching, and runoff after field application. Herbicide residues in the environment pose potential risks to ecological safety and human health. Therefore, establishing analytical methods to determine herbicide residues in environmental samples is of great importance. In this study, an analytical method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive electrospray ionization mode (ESI+) was developed for the determination of isoxaflutole, metazachlor, and saflufenacil residues in soil, sediment, and water. The instrumental detection parameters, including electrospray ionization mode, mobile phase, and chromatographic column, were optimized. The mobile phases were methanol (A) and 0.1% formic acid aqueous solution (B). Gradient elution was performed as follows: 0-1.0 min, 60%A; 1.0-2.0 min, 60%A-90%A; 2.0-3.0 min, 90%A; 3.0-4.0 min, 90%A-60%A; 4.0-5.0 min, 60%A. The samples were salted after extraction with acetonitrile and cleaned using a C18 solid-phase extraction column. Different solid-phase extraction columns and leaching conditions were investigated during sample pretreatment. Working curves in the neat solvent and matrix were constructed by plotting the measured peak areas as a function of the concentrations of the analytes in the neat solvent and matrix. Good linearities were found for isoxaflutole, metazachlor, and saflufenacil in the solvent and matrix-matched standards in the range of 0.0005-0.02 mg/L, with r≥0.9961. The matrix effects of the three herbicides in soil, sediment, and water ranged from -10.1% to 16.5%. The limits of detection (LODs, S/N=3) for isoxaflutole, metazachlor, and saflufenacil were 0.05, 0.01, and 0.02 µg/kg, respectively. The limits of quantification (LOQs, S/N=10) for isoxaflutole, metazachlor, and saflufenacil were 0.2, 0.05, and 0.05 µg/kg, respectively. The herbicides were applied to soil, sediment, and water at spiked levels of 0.005, 0.1, and 2.0 mg/kg, respectively. The average recoveries for isoxaflutole, metazachlor, and saflufenacil in soil, sediment, and water were in the ranges of 77.2%-101.9%, 77.9%-105.1%, and 80.8%-107.1%, respectively. The RSDs for isoxaflutole, metazachlor, and saflufenacil were in the ranges of 1.4%-12.8%, 1.2%-7.7%, and 1.5%-11.5%, respectively. The established method was used to analyze actual samples collected from four different sites in Zhejiang Province (Xiaoshan, Taizhou, Dongyang, and Yuhang) and one site in Heilongjiang (Jiamusi). The proposed method is simple, rapid, accurate, stable, and highly practical. It can be used to detect isoxaflutole, metazachlor, and saflufenacil residues in soil, sediment, and water and provides a reference for monitoring the residual pollution and environmental behavior of herbicides.

Determination of 4-chloro-2-methylphenoxyacetic acid residues in wheat and soil by ultra-performance liquid chromatography/tandem mass spectrometry.

A rapid, highly sensitive, and selective method was developed for the identification and quantitation of the herbicide 4-chloro-2-methylphenoxyacetic acid (MCPA) in wheat plants, wheat grain, and soil by ultra-performance LC/MS/MS. MCPA was extracted from the sample (5 or 10 g) with acetonitrile, and an aliquot was taken for cleanup with primary secondary amine. Two precursor product ion transitions for MCPA were measured and evaluated to provide maximum confidence in the results. Average recoveries from wheat plants, wheat grain, and soil fortified at levels of 0.01-1.0 mg/kg ranged from 75.1 to 93.9%, with RSD(r) values of 3.0-9.3% and RSDR values of 3.1-8.7%. Coefficients of determination of R2 > or = 0.9994 were obtained for wheat and soil matrix calibration curves at MCPA levels of 0.01-5.0 microg/mL. Under conditions of electrospray ionization in the negative-ion mode, the ion at m/z 141 was monitored for quantitation; the parent ion at m/z 199 was also measured. The LOD values for MCPA in wheat plants, wheat grain, and soil were determined to be 0.005, 0.004, and 0.004 mg/kg, respectively, and corresponding LOQ values were 0.02, 0.01, and 0.01 mg/kg. This method can be used to determinate MCPA residues in wheat products and soils.

[Effects of chlorimuron-ethyl on soil microbial community structure in soybean field].

By using phospholipid fatty acids (PLFA) method, this paper studied the soil microbial community structure in the soybean fields with different chlorimuron-ethyl application history in Weihe district of Heilongjiang Province. In the meantime, the residual amount of chlorimuron-ethyl in soil was determined. There was a very low residual of chlorimuron-ethyl in soil under the conditions of different chlorimuron-ethyl application history. With the increasing year of chlorimuron-ethyl application, the total concentration of soil microbial PLFA and the ratios of fungi/bacteria and Gram negative/Gram positive bacteria decreased, and the microbial stress level increased. Principal component analysis (PCA) showed that long-term application of chlorimuron-ethyl into soybean field changed the soil microbial community structure significantly.

Genistein-3'-sulfonic acid dihydrate.

IN THE TITLE COMPOUND [SYSTEMATIC NAME: 5-(5,7-dihydr-oxy-4-oxo-4H-chromen-yl)-2-hydroxy-benzene-sulfonic acid dihydrate], C(15)H(10)O(8)S·2H(2)O, the benzopyran-one ring is not coplanar with the phenyl ring, the dihedral angle between them being 41.35 (3)°. No H atom was placed on the sulphonic acid group because it was not possible to distinguish between the two S=O bonds and the S-O bond. In the crystal, the mol-ecules are linked by classical O-H⋯O and C-H⋯O intra- and inter-molecular hydrogen bonds and aromatic π-π stacking inter-actions [centroid-centroid distance of 3.4523 (14) Šbetween the 1, 4-pyran-one rings and the benzene rings, and 3.6337 (14) Šbetween the benzene rings] into a supra-molecular structure.