Zhang Haizhen, Huang Min, Yu Weiwei, Zhang A'wei, Zhang Kankan, Hu Deyu
State Key Laboratory Breeding Base of Green Pesticide and Agricultural Bioengineering, Key Laboratory of Green Pesticide and Agricultural Bioengineering, Ministry of Education, Guizhou University, Guiyang, China.
Biomed Chromatogr. 2018 Jul;32(7):e4230. doi: 10.1002/bmc.4230. Epub 2018 Apr 2.
A simple and rapid method for enantioselective determination of dufulin in cucumber and soil was developed by liquid chromatography with tandem mass spectrometry. The enantiomers were separated on a Superchiral S-OD chiral cellulose tris(3,5-dimethylphenylcarbamate) column at 20°C, with a mixture of acetonitrile and water (0.1% formic acid; 52:48, v/v) as mobile phase at a flow rate of 0.65 mL/min. The pretreatment conditions were optimized using an orthogonal test, and the optimized method showed good linearity and sensitivity. The limits of detection and limits of quantification of two dufulin enantiomers were 0.006 and 0.02 mg/kg, respectively. The average recoveries of S-enantiomer and R-enantiomer in cucumber and soil were 80.61-99.83% and 80.97-102.96%, respectively, with relative standard deviations of 1.30-9.72%. The method was successfully applied to determine dufulin in real cucumber and soil samples. The results demonstrate that the method could facilitate further research on the differences between individual dufulin enantiomers with respect to metabolites and environmental fate and finally help reveal the complex interactions that exist between dufulin, humans and the environment.
建立了一种采用液相色谱-串联质谱法对黄瓜和土壤中杜氟灵进行对映体选择性测定的简单快速方法。对映体在Superchiral S-OD手性纤维素三(3,5-二甲基苯基氨基甲酸酯)柱上于20℃分离,以乙腈和水(0.1%甲酸;52:48,v/v)的混合物作为流动相,流速为0.65 mL/min。采用正交试验对预处理条件进行了优化,优化后的方法具有良好的线性和灵敏度。两种杜氟灵对映体的检测限和定量限分别为0.006和0.02 mg/kg。黄瓜和土壤中S-对映体和R-对映体的平均回收率分别为80.61 - 99.83%和80.97 - 102.96%,相对标准偏差为1.30 - 9.72%。该方法成功应用于实际黄瓜和土壤样品中杜氟灵的测定。结果表明,该方法有助于进一步研究杜氟灵对映体在代谢产物和环境归宿方面的差异,最终有助于揭示杜氟灵、人类和环境之间存在的复杂相互作用。