Liang Weiqian, Wang Juntao, Zang Xiaohuan, Dong Wenhuan, Wang Chun, Wang Zhi
College of Science, Hebei Agricultural University, Baoding 071001, China.
College of Science, Hebei Agricultural University, Baoding 071001, China.
J Chromatogr A. 2017 Mar 31;1491:9-15. doi: 10.1016/j.chroma.2017.02.034. Epub 2017 Feb 20.
In this work, a barley husk biomaterial was successfully carbonized by hydrothermal method. The carbon had a high specific surface area and good stability. It was coated onto a stainless steel wire through sol-gel technique to prepare a solid-phase microextraction fiber for the extraction of trace levels of twelve pesticides (tsumacide, fenobucarb, indoxacarb, diethofencarb, thimet, terbufos, malathion, thiamethoxam, imidacloprid, buprofezin, acetamiprid, thiamethoxam) from vegetable samples prior to gas chromatography-mass spectrometric (GC-MS) detection. The main experimental parameters that could influence the extraction efficiency such as extraction time, extraction temperature, sample pH, sample salinity, stirring rate, desorption temperature and desorption time, were investigated. Under the optimized conditions, the linearity was observed in the range of 0.2-75.0μgkg for tomato samples, and 0.3-60.0μgkg for cucumber samples, with the correlation coefficients (r) ranging from 0.9959 to 0.9983. The limits of detection of the method were 0.01-0.05μgkg for tomato samples, and 0.03-0.10μgkg for cucumber samples. The recoveries of the analytes for the method from spiked samples were in the range of 76%-104%, and the precision, expressed as the relative standard deviations, was less than 12%.
在本研究中,通过水热法成功地将大麦壳生物材料碳化。所得碳材料具有高比表面积和良好的稳定性。通过溶胶 - 凝胶技术将其涂覆在不锈钢丝上,制备了一种固相微萃取纤维,用于在气相色谱 - 质谱(GC - MS)检测之前从蔬菜样品中萃取痕量的十二种农药(杀螨酯、仲丁威、茚虫威、乙霉威、甲基异柳磷、特丁硫磷、马拉硫磷、噻虫嗪、吡虫啉、噻嗪酮、啶虫脒、噻虫嗪)。研究了可能影响萃取效率的主要实验参数,如萃取时间、萃取温度、样品pH值、样品盐度、搅拌速率、解吸温度和解吸时间。在优化条件下,番茄样品在0.2 - 75.0μg/kg范围内呈线性,黄瓜样品在0.3 - 60.0μg/kg范围内呈线性,相关系数(r)在0.9959至0.9983之间。该方法对番茄样品的检测限为0.01 - 0.05μg/kg,对黄瓜样品的检测限为0.03 - 0.10μg/kg。加标样品中分析物的回收率在76% - 104%范围内,以相对标准偏差表示的精密度小于12%。