Page 54 - 《精细化工》2023年第11期
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第 40 卷第 11 期                            精   细   化   工                                 Vol.40, No.11
             2 023 年 11 月                            FINE CHEMICALS                                 Nov.  2023


              功能材料
                                基于纤维素基固相萃取材料分析


                                          尿液中的苯丙胺毒品



                                                                                    1*
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                                                                       1
                                   罗   竞    1,2 ,王璐颖 ,刘以凡 ,林春香
                 (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)

                 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 0.08 L/g(萃取剂)、洗脱时间为 20 min 的最佳条件下,该法的线性范围为 0.01~2.00 mg/L
                    2
                 (R =0.9973),检出限为 2.5 μg/L,定量限为 8.0 μg/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%。
                 关键词:纤维素;苯丙胺;固相萃取;高效液相色谱法;功能材料
                 中图分类号:O658.2;R446.12      文献标识码:A      文章编号:1003-5214 (2023) 11-2366-10


                             Analysis of amphetamine in urine by cellulose-based

                                          solid phase extraction material


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                                                                                      1*
                                           1,2
                                  LUO Jing , WANG Luying , LIU Yifan , LIN Chunxiang
                 (1.  College of Environmental  &  Safety Engineering, Fuzhou  University, Fuzhou  350108, Fujian, China; 2.  Fujian
                 Huaxia Energy Design and Research Institute Co., Ltd., Fuzhou 350003, Fujian, China)
                 Abstract: 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
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                 0.01~2.00 mg/L (R =0.9973), and the limit of detection was 2.5 μg/L with the quantification limit of 8.0 μg/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%.

                 收稿日期:2023-03-13;  定用日期:2023-06-21; DOI: 10.13550/j.jxhg.20230201
                 基金项目:国家自然科学基金项目(22208057);福建省自然科学基金项目(2020J01506)
                 作者简介:罗   竞(1990—),男,硕士,高级工程师,E-mail:351823675@qq.com。联系人:林春香(1982—),女,博士,教授,
                 E-mail:lcx2010@fzu.edu.cn。
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