Institute of Quality and Standard for Agro-products, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China.
J Agric Food Chem. 2012 Oct 17;60(41):10188-95. doi: 10.1021/jf302620s. Epub 2012 Oct 8.
An enantioselective method is presented for the determination of isocarbophos in soil by liquid chromatography coupled with tandem mass spectrometry. The pesticide residues in soil samples were extracted with acetonitrile, and complete enantioseparation was obtained on an amylose tris(3,5-dimethylphenylcarbamate) chiral column using acetonitrile/2 mM ammonium acetate solution containing 0.1% formic acid (60:40, v/v) as the mobile phase. The absolute configuration of isocarbophos enantiomers was determined by the combination of experimental and calculated electronic circular dichroism spectra. The method was utilized to investigate the degradation of isocarbophos in soils (Changchun, Hangzhou, and Zhengzhou) under sterilized or native conditions. Isocarbophos enantiomers were configurationally stable in the selected soils, and the pesticide degradation was not enantioselective in the sterilized condition. The degradation behavior of rac-isocarbophos was different under native conditions, with no enantioselectivity in the Changchun soil and with the S-(+)-isocarbophos enriched in the Hangzhou and Zhengzhou soils.
本文建立了一种用手性液相色谱-串联质谱测定土壤中异稻瘟净对映体残留的分析方法。采用乙腈提取土壤中的农药残留,在氨基糖三(3,5-二甲苯基氨基甲酸酯)手性柱上,以乙腈/2mM 乙酸铵溶液(含 0.1%甲酸,60:40,v/v)为流动相,实现了对映体的完全拆分。利用实验和计算电子圆二色谱相结合的方法确定了异稻瘟净对映体的绝对构型。采用该方法研究了异稻瘟净在长春、杭州和郑州土壤中(灭菌和非灭菌条件下)的降解情况。结果表明,在所选土壤中,异稻瘟净对映体构型稳定,灭菌条件下农药降解没有对映体选择性,而非灭菌条件下 rac-异稻瘟净的降解行为不同,在长春土壤中没有对映体选择性,而在杭州和郑州土壤中则富集了 S-(+)-异稻瘟净。