柚子皮制备磁性生物炭的表征及其对水中氯胺酮的检测 |
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基金项目:社会事业与民生保障科技创新专项(2021(农社)13);重庆市教委重点项目(KJZD-K202100301);“成渝地区双城经济圈建设”科技创新项目(KJCXZD2020016) |
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中文摘要:该研究以柚子皮为原料,制备了性能优良的磁性生物炭吸附剂,建立了快速检测氯胺酮的磁性固相萃取/超高效液相色谱-串联质谱法。扫描电镜和振动样品磁强计表征结果表明成功合成了磁性生物炭。采用单因素实验优化了吸附剂用量、吸附时间、溶液pH值,并采用Box-Behnken设计实验考察了解吸剂比例、解吸体积、解吸时间对水中氯胺酮回收率的影响。结果表明,在1 ~ 100 μg·L-1范围内,氯胺酮标准曲线的相关系数r > 0.999,检出限为0.263 μg·L-1,定量下限为0.878 μg·L-1。方法在不同水样中的加标回收率为84.0% ~ 99.9%,日内和日间相对标准偏差分别为0.40% ~ 3.4%和0.25% ~ 1.9%。所建立的方法操作简便,准确高效,灵敏度高,适用于水中氯胺酮的检测。 |
中文关键词:磁性生物炭 超高效液相色谱-串联质谱 氯胺酮 吸附 水 |
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Characterization of Magnetic Biochar Prepared with Pomelo Peel and Its Application in Detection of Ketamine in Water |
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Abstract:In this study,an ultra-high performance liquid chromatography-tandem mass spectrometry for the rapid detection of ketamine in water was established,based on a magnetic solid-phase extraction technique with magnetic biochar as adsorbent.The magnetic biochar composites with excellent adsorption performance were prepared using the low-cost,environmentally friendly and renewable pomelo peels as biomass raw material,so as to achieve the efficient enrichment and purification of ketamine in water.The characterization results of scanning electron microscope and vibrating sample magnetometer both indicated that the magnetic biochar was successfully synthesized.The sample pretreatment conditions were optimized in detail.Single factor experiments were firstly used to optimize the experimental parameters affecting the extraction efficiency such as the dosage of adsorbent,adsorption time and pH value of solution.Box-Behnken design was further applied to investigate the effects of adsorbent proportion,desorption volume and desorption time on the recovery of ketamine in water.The results revealed that there was good linear relationship for ketamine in the concentration range of 1-100 μg·L-1 under optimal conditions,with correlation coefficient(r) larger than 0.999.The limit of detection of the method was 0.263 μg·L-1,and the limit of quantification was 0.878 μg·L-1.In different actual water samples,the recoveries at four spiked levels of 1,10,20 and 50 μg·L-1 ranged from 84.0% to 99.9%,with intra-day and inter-day relative standard deviations of 0.40%-3.4% and 0.25%-1.9%,respectively.The established method possesses the advantages of easy operation,high efficiency,accuracy,and sensitivity,which is suitable for the detection of ketamine in water. |
Key Words:magnetic biochar ultra-high performance liquid chromatography-mass spectrometry ketamine adsorption water |
引用本文:马双,游嘉德,巫端浩,江茉莉,周琴,曹淑瑞.柚子皮制备磁性生物炭的表征及其对水中氯胺酮的检测[J].分析测试学报,2022,41(11):1671-1677. |
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