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用于微固相萃取的分子印迹聚合物-溶胶-凝胶片剂:II. 采用液相色谱-串联质谱法测定人尿液样本中的苯丙胺

Molecularly imprinted polymer-sol-gel tablet toward micro-solid phase extraction: II. Determination of amphetamine in human urine samples by liquid chromatography-tandem mass spectrometry.

作者信息

El-Beqqali Aziza, Andersson Lars I, Jeppsson Amin Dadoun, Abdel-Rehim Mohamed

机构信息

Department of Environmental Sci. & Analytical Chemistry, Stockholm University, SE10691 Stockholm, Sweden.

Department of Laboratory Medicine, Karolinska Institutet, Stockholm, Sweden.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Sep 15;1063:130-135. doi: 10.1016/j.jchromb.2017.08.027. Epub 2017 Aug 26.

Abstract

Amphetamine selective molecularly imprinted sol-gel polymer tablets, MIP-tablets, for solid-phase microextraction of biofluid samples were prepared. An acetonitrile solution of deuterated amphetamine template and silane precursor, 3-(propylmethacrylate) trimethoxysilane, was soaked into the pores of polyethylene tablet substrates and polymerized by an acid-catalysed sol-gel process. Application of the resultant MIP-tablets to extract amphetamine from human urine samples followed by LC-MS/MS analysis was investigated. The extraction protocol was optimised with respect to pH of sample, addition of sodium chloride, extraction time, desorption solvent and desorption time. The final analysis method determined amphetamine in human urine with a limit of detection (LOD) of 1.0ng/mL and a lower limit of quantification (LLOQ) of 5ng/mL. Validation demonstrated accuracy of the method was 91.0-104.0% and inter-assay precision was 4.8-8.5% (RSD). Extraction recovery was 80%. The MIP-tablets could be re-used and the same tablet could be employed for more than twenty extractions.

摘要

制备了用于生物流体样品固相微萃取的苯丙胺选择性分子印迹溶胶-凝胶聚合物片剂(MIP-片剂)。将氘代苯丙胺模板和硅烷前驱体3-(甲基丙烯酸丙酯)三甲氧基硅烷的乙腈溶液浸泡到聚乙烯片剂基质的孔中,并通过酸催化溶胶-凝胶过程进行聚合。研究了所得MIP-片剂用于从人尿液样品中萃取苯丙胺,随后进行液相色谱-串联质谱(LC-MS/MS)分析的情况。针对样品pH值、氯化钠添加量、萃取时间、解吸溶剂和解吸时间对萃取方案进行了优化。最终的分析方法测定人尿液中苯丙胺的检测限(LOD)为1.0 ng/mL,定量下限(LLOQ)为5 ng/mL。验证表明该方法的准确度为91.0 - 104.0%,批间精密度为4.8 - 8.5%(相对标准偏差)。萃取回收率为80%。MIP-片剂可重复使用,同一片剂可用于二十多次萃取。

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