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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
Journal of Chromatography B ( IF 3 ) Pub Date : 2017-08-26 , DOI: 10.1016/j.jchromb.2017.08.027
Aziza El-Beqqali , Lars I. Andersson , Amin Dadoun Jeppsson , Mohamed Abdel-Rehim

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 1.0 ng/mL and a lower limit of quantification (LLOQ) of 5 ng/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.



中文翻译:

分子印迹聚合物溶胶凝胶片用于微固相萃取:II。液相色谱-串联质谱法测定人尿液中的苯丙胺

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。将氘化的苯丙胺模板和硅烷前体3-(甲基丙烯酸丙酯)三甲氧基硅烷的乙腈溶液浸入聚乙烯片剂基材的孔中,并通过酸催化的溶胶-凝胶法进行聚合。研究了由此产生的MIP片剂从人尿液样品中提取苯丙胺,然后进行了LC-MS / MS分析。针对样品的pH,氯化钠的添加,萃取时间,脱附溶剂和脱附时间对萃取方案进行了优化。最终分析方法测定了人尿中的苯丙胺,其检出限(LOD)为1.0 ng / mL,定量下限(LLOQ)为5 ng / mL。验证表明,该方法的准确性为91.0–104.0%,批间分析的准确性为4.8–8.5%(RSD)。提取回收率为80%。MIP片剂可以重复使用,同一块片剂可以用于20多次提取。

更新日期:2017-08-26
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