基于聚乙烯亚胺修饰磁性纳米粒的分散固相萃取/高效液相色谱法测定水中非甾体抗炎药  

Determination of non-steroidal anti-inflammatory drugs in the environmental water samples by a polyvinylimide-modified magnetic nanoparticles-based solid phase extraction coupled with high-performance liquid chromatography

作　　者：汤晓航 宋会林 姚丽莹 秦国文 王星晨 柳文媛[2] 纪顺利 TANG Xiaohang;SONG Huilin;YAO Liying;QIN Guowen;WANG Xingchen;LIU Wenyuan;JI Shunli(Department of Pharmacy,Dongtai People's Hospital,Dongtai 22420;School of Pharmacy,China Pharmaceutical University,Nanjing 210009;Wuhu Institute of Technology,Wuhu Life and Health Research Center,Wuhu 241000,China)

机构地区：[1]东台市人民医院药学科,东台224200 [2]中国药科大学药学院,南京210009 [3]芜湖职业技术学院,芜湖生命健康研究中心,芜湖241000

出　　处：《中国药科大学学报》2024年第4期485-492,共8页Journal of China Pharmaceutical University

基　　金：国家自然科学基金项目(No.81703472);安徽省高等学校自然科学类研究项目(No.2023AH052394)。

摘　　要：环境水样中非甾体抗炎药(NSAIDs)的长期存在不仅会影响水生生物的生命安全,扰乱生态系统环境,而且会对人类健康构成严重威胁。采用溶剂热法首先制备了氨基功能化Fe_(3)O_(4)纳米粒子(Fe_(3)O_(4)-NH_(2))。随后,通过室温下水溶液中的席夫碱反应,以戊二醛为交联剂,将具有支链结构的聚乙烯亚胺(PEI)成功地接枝到Fe_(3)O_(4)纳米粒子上,合成了一种可回收的PEI接枝磁性纳米吸附剂(Fe_(3)O_(4)@PEI)并将其应用于环境水中NSAIDs的检测。通过各种表征手段研究了Fe_(3)O_(4)@PEI的组成特性,并对影响NSAIDs萃取效果的参数进行了优化。Fe_(3)O_(4)@PEI对4种NSAIDs具有高吸附性,与高效液相色谱联用可对环境水样中的酮洛芬、萘普生、双氯芬酸和托芬那酸4种NSAIDs进行定量分析,在1~500μg/mL范围内,色谱峰面积与质量浓度呈良好的线性关系,样品在3种不同添加水平下的加标回收率在85.6%~107.8%,日内精密度均小于7.8%(n=6),日间精密度均小于9.5%(n=3)。该方法操作简单、准确高效,可用于环境水样中非甾体抗炎药的测定。The long-term presence of non-steroidal anti-inflammatory drugs(NSAIDs)in the environmental water samples not only affects the life safety of aquatic organisms and disturbs the ecoenvironment,but also poses a serious threat to human health.In this study,amino-functionalized Fe_(3)O_(4)nanoparticles(Fe_(3)O_(4)-NH_(2))were firstly prepared by solvothermal method.Subsequently,polyethyleneimine(PEI)with a branched chain structure was successfully grafted onto Fe_(3)O_(4)nanoparticles by Schiff base reaction in aqueous solution at room temperature using glutaraldehyde as a cross-linking agent,and a recyclable PEI-grafted magnetic nano-sorbent(Fe_(3)O_(4)@PEI)was synthesized and applied for the detection of NSAIDs in the environmental water samples.The compositional properties of Fe_(3)O_(4)@PEI were investigated by different characterization methods and the parameters affecting the extraction of NSAIDs were optimized.Due to high adsorption of Fe_(3)O_(4)@PEI for NSAIDs,the quantitative analysis of four NSAIDs in the environmental water samples,ketoprofen,naproxen,diclofenac and tolfenamic acid,was performed in combination with high-performance liquid chromatography.A good linear relationship between the chromatographic peak area and concentration was observed in the range of 1−500μg/mL.The recoveries of the samples at three different spiked levels ranged from 85.6%to 107.8%;the intra-day precision was less than 7.8%(n=6);and the inter-day precision was less than 9.5%(n=3).The method is simple,rapid,accurate and reliable,and can be used for the analysis of NSAIDs in the environmental water samples.

关 键 词：非甾体抗炎药 聚乙烯亚胺 磁性固相萃取 纳米粒 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]