College of Environmental and Safety Engineering,Fuzhou University
Natural Science Foudation of China(22208057)；Natural Science Foudation of Fujian Province(2020J01506)
以纤维素为原料，通过酸酐改性制备纤维素基萃取材料（Cell-COOH），用于尿液中苯丙胺的富集，并建立基于该材料的固相萃取-高效液相色谱联用用于尿液中苯丙胺的测定。采用现代分析测试手段对Cell-COOH结构进行表征；优化固相萃取条件，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，该方法表现出良好的特异性和抗干扰能力，经过7次循环使用后萃取效率仍保持在92%以上。在最佳萃取条件下，该方法的线性范围为0.01~2 mg/L（R2=0.9973%），检出限为2.5 μg/L，定量限为8 μg/L。使用Cell-COOH对实际尿液中的苯丙胺进行萃取，其回收率为74.41~82.14%，相对偏差（n=3）为2.32~6.85%。
Cellulose-based extraction material (Cell-COOH) was prepared from cellulose using acid anhydride modification for the enrichment of amphetamine in urine, and a solid-phase extraction coupled with high performance liquid chromatography based on Cell-COOH was established for the determination of amphetamine drugs in urine. The structure of Cell-COOH was characterized by modern analytical methods. Solid-phase extraction conditions were also optimized. Specificity, interference resistance and reusability of Cell-COOH were tested, and the feasibility of the method was verified. The results showed that the surface of Cell-COOH contained carboxyl functional group, showing 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% after seven cycles of use. Under the optimal extraction conditions, the linear range of the method was among 0.01~2 mg/L (R2=0.9973%), and the limit of detection was 2.5 μg/L with the quantification limit of 8 μg/L. The recovery rate of amphetamine could reach 74.41~82.14% when using Cell-COOH as solid phase extractant in actual urine, and the relative deviation at the 3 spiked levels was 2.32~6.85%.