Tianjin Key Laboratory of Organic Solar Cells and Photochemical Conversion, School of Chemistry and Chemical Engineering, Tianjin University of Technology, Tianjin, China.
J Sep Sci. 2017 Oct;40(20):3938-3945. doi: 10.1002/jssc.201700594. Epub 2017 Sep 5.
Sulfonated poly(styrene-divinylbenzene) modified with five kinds of amine functional groups was applied to the determination of carbendazim in apple samples with a pipette-tip solid-phase extraction method. The structures of the polymers were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis. Five different modifications of the solid-phase extraction sorbent based on sulfonated poly(styrene-divinylbenzene) were tested under static and pipette-tip solid-phase extraction conditions. The polymer modified with p-methoxyaniline showed the best recognition capacity and adsorption amount for carbendazim. Under the optimum conditions, 3.00 mg of the adsorbent, 1.00 mL of ethyl acetate as washing solvent, and 1.00 mL of ammonia/acetonitrile (5:95, v/v) as elution solvent were used in the pretreatment procedure of apple samples. The calibration graphs of carbendazim in methanol were linear over 5.00-200.00 μg/mL, and the limits of detection and quantification were 0.01 and 0.03 μg/mL, respectively. The method recoveries of carbendazim were in the range of 91.31-98.13% with associated intraday relative standard deviations of 0.76-2.13% and interday relative standard deviations of 1.10-1.85%. Sulfonated poly(styrene-divinylbenzene) modified with p-methoxyaniline showed satisfactory results (recovery: 97.96%) and potential for the rapid purification of carbendazim in apple samples combined with the pipette-tip solid-phase extraction.
用 5 种胺官能团磺化的聚苯乙烯-二乙烯基苯改性物，采用微量进样固相萃取法测定苹果样品中的多菌灵。采用扫描电子显微镜、傅里叶变换红外光谱和热重分析对聚合物的结构进行了表征。在静态和微量进样固相萃取条件下，测试了基于磺化聚苯乙烯-二乙烯基苯的 5 种不同的固相萃取吸附剂的改性。经甲氧基苯胺改性的聚合物对多菌灵表现出最佳的识别能力和吸附量。在最佳条件下，用 3.00 mg 吸附剂、1.00 mL 乙酸乙酯作为洗涤溶剂、1.00 mL 氨/乙腈（5:95，v/v）作为洗脱溶剂，对苹果样品进行预处理。甲醇中多菌灵的校准曲线在 5.00-200.00 μg/mL 范围内呈线性，检测限和定量限分别为 0.01 和 0.03 μg/mL。多菌灵的方法回收率在 91.31-98.13%范围内，日内相对标准偏差为 0.76-2.13%，日间相对标准偏差为 1.10-1.85%。经甲氧基苯胺改性的磺化聚苯乙烯-二乙烯基苯结合微量进样固相萃取，对苹果样品中多菌灵的快速净化具有令人满意的效果（回收率：97.96%）和潜力。
