1.重庆化工职业学院 环境与质量检测学院,重庆 401228
2.西南政法大学 司法鉴定中心,重庆 401120
3.长江师范学院 现代农业与生物工程学院,重庆 408100
曹淑瑞,博士,教授级高级工程师,研究方向:纳米材料与物证技术,E - mail:caoshurui@yeah.net
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马双,游嘉德,巫端浩等.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.
MA Shuang,YOU Jia-de,WU Duan-hao,et al.Characterization of Magnetic Biochar Prepared with Pomelo Peel and Its Application in Detection of Ketamine in Water[J].Journal of Instrumental Analysis,2022,41(11):1671-1677.
马双,游嘉德,巫端浩等.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. DOI: 10.19969/j.fxcsxb.22052601.
MA Shuang,YOU Jia-de,WU Duan-hao,et al.Characterization of Magnetic Biochar Prepared with Pomelo Peel and Its Application in Detection of Ketamine in Water[J].Journal of Instrumental Analysis,2022,41(11):1671-1677. DOI: 10.19969/j.fxcsxb.22052601.
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。
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.
磁性生物炭超高效液相色谱-串联质谱氯胺酮吸附水
magnetic biocharultra-high performance liquid chromatography-mass spectrometryketamineadsorptionwater
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