Liu Qianjun, Chen Di, Wu Jiyuan, Yin Guangcai, Lin Qintie, Zhang Min, Hu Huawen
College of Environmental Science and Engineering, Guangdong University of Technology, Guangzhou, P. R. China.
School of Materials Science and Energy Engineering, Foshan University, Foshan, P. R. China.
J Sep Sci. 2018 Apr;41(8):1812-1820. doi: 10.1002/jssc.201701126. Epub 2018 Feb 9.
A quick, easy, cheap, effective, rugged, and safe procedure was designed to extract pesticide residues from fruits and vegetables with a high percentage of water. It has not been used extensively for the extraction of phthalate esters from sediments, soils, and sludges. In this work, this procedure was combined with gas chromatography with mass spectrometry to determine 16 selected phthalate esters in soil. The extraction efficiency of the samples was improved by ultrasonic extraction and dissolution of the soil samples in ultra-pure water, which promoted the dispersion of the samples. Furthermore, we have simplified the extraction step and reduced the risk of organic solvent contamination by minimizing the use of organic solvents. Different extraction solvents and clean-up adsorbents were compared to optimize the procedure. Dichloromethane/n-hexane (1:1, v/v) and n-hexane/acetone (1:1, v/v) were selected as the extractants from the six extraction solvents tested. C18/primary secondary amine (1:1, m/m) was selected as the sorbent from the five clean-up adsorbents tested. The recoveries from the spiked soils ranged from 70.00 to 117.90% with relative standard deviation values of 0.67-4.62%. The proposed approach was satisfactorily applied for the determination of phthalate esters in 12 contaminated soil samples.
设计了一种快速、简便、廉价、有效、耐用且安全的方法，用于从含水量高的水果和蔬菜中提取农药残留。该方法尚未广泛用于从沉积物、土壤和污泥中提取邻苯二甲酸酯。在本研究中，将该方法与气相色谱-质谱联用，以测定土壤中16种选定的邻苯二甲酸酯。通过超声提取以及将土壤样品溶解于超纯水中提高了样品的提取效率，这促进了样品的分散。此外，我们简化了提取步骤，并通过尽量减少有机溶剂的使用降低了有机溶剂污染的风险。比较了不同的提取溶剂和净化吸附剂以优化该方法。从六种测试提取溶剂中选择二氯甲烷/正己烷（1:1，v/v）和正己烷/丙酮（1:1，v/v）作为提取剂。从五种测试净化吸附剂中选择C18/伯仲胺（1:1，m/m）作为吸附剂。加标土壤的回收率在70.00%至117.90%之间，相对标准偏差值为0.67 - 4.62%。所提出的方法成功应用于12个受污染土壤样品中邻苯二甲酸酯的测定。
