基于纤维素基固相萃取材料分析尿液中的苯丙胺毒品  

Analysis of amphetamine in urine by cellulose-based solid phase extraction material

作　　者：罗竞 王璐颖 刘以凡[1] 林春香[1] LUO Jing;WANG Luying;LIU Yifan;LIN Chunxiang(College of Environmental&Safety Engineering,Fuzhou University,Fuzhou 350108,Fujian,China;Fujian Huaxia Energy Design and Research Institute Co.,Ltd.,Fuzhou 350003,Fujian,China)

机构地区：[1]福州大学环境与安全工程学院,福建福州350108 [2]福建省华厦能源设计研究院有限公司,福建福州350003

出　　处：《精细化工》2023年第11期2366-2375,2393,共11页Fine Chemicals

基　　金：国家自然科学基金项目(22208057);福建省自然科学基金项目(2020J01506)。

摘　　要：对纤维素进行酸酐改性,制备了纤维素基萃取材料(Cell-COOH),用于尿液中苯丙胺的富集,并建立了基于该材料的固相萃取-高效液相色谱联用技术,用于尿液中苯丙胺的测定。采用FTIR、XRD、SEM、XPS对Cell-COOH结构进行了表征;优化了固相萃取条件,并对其特异性、抗干扰能力、可重复利用性及方法的可行性进行了测试和验证。结果表明,Cell-COOH表面含有羧基官能团,对苯丙胺具有较好的吸附能力;在其他滥用药物和共存离子的干扰下,该法表现出良好的特异性和抗干扰能力,在第7次使用时萃取回收率仍保持在92%以上。在pH为8,萃取剂Cell-COOH用量为0.50 g/L,萃取时间为30 min,洗脱剂为体积分数0.8%的盐酸、洗脱剂用量为0.08L/g(萃取剂)、洗脱时间为20min的最佳条件下,该法的线性范围为0.01~2.00mg/L(R^(2)=0.9973),检出限为2.5μg/L,定量限为8.0μg/L。使用Cell-COOH对实际尿液中的苯丙胺进行了萃取,其萃取回收率为74.41%~82.14%,相对标准偏差(n=3)为2.32%~6.85%。Cellulose-based extraction material(Cell-COOH)was prepared from cellulose modification with acid anhydride for amphetamine enrichment in urine,and characterized by FTIR,XRD,SEM and XPS.A solid-phase extraction technique coupled with high performance liquid chromatography based on Cell-COOH was established for the determination of amphetamine in urine.The solid-phase extraction conditions were then optimized,while the interference resistance and reusability of Cell-COOH were evaluated and the feasibility of this technique was verified.The results showed that the surface of Cell-COOH contained carboxyl functional group with good adsorption to amphetamine.The method showed good specificity and anti-interference ability under the interference of other abused drugs and urine co-existing ions,and the extraction efficiency could remain above 92%when used for the seventh time.Under the optimal extraction conditions of pH=8,extractant dosage 0.50 g/L,extraction time 30 min,eluent of 0.8%(volume fraction)hydrochloric acid,eluent dosage 0.08 L/g,elution time 20 min,the linear range of the method was among 0.01~2.00 mg/L(R^(2)=0.9973),and the limit of detection was 2.5μg/L with the quantification limit of 8.0μg/L.The extraction recovery of amphetamine could reach 74.41%~82.14%when using Cell-COOH as solid phase extractant in actual urine,with the relative deviation(n=3)of 2.32%~6.85%.

关 键 词：纤维素 苯丙胺 固相萃取 高效液相色谱法 功能材料 

分 类 号：O658.2[理学—分析化学] R446.12[理学—化学]