Chapuis-Hugon Florence, Cruz-Vera Marta, Savane Ramatoulaye, Ali Wassim Hadj, Valcarcel Miguel, Deveaux Marc, Pichon Valerie
Department of Environmental and Analytical Chemistry UMR PECSA 7195, Ecole Supérieure de Physique et de Chimie Industrielles (ESPCI), Paris, France.
J Sep Sci. 2009 Oct;32(19):3301-9. doi: 10.1002/jssc.200900247.
For the first time, a molecularly imprinted polymer (MIP) was synthesized by a noncovalent imprinting approach for the selective extraction of an illicit drug, LSD, from hair and urine samples. For the synthesis of MIP, an analog of LSD, was taken as a dummy template, methacrylic acid as a functional monomer, and ACN as a porogen solvent. The MIP was used for offline extraction before HPLC-MS analysis. By studying the interactions taking place between the LSD and the MIP, a selective procedure was established in organic media and applied to hair samples. By this way, 0.1 ng/mg of LSD was successfully detected in hair with 82% of extraction recovery. A low retention was also obtained on the control polymer (only 9%). This procedure was then modified to obtain a selective extraction in aqueous media for the determination of LSD in urine samples. The comparison with a conventional C18 clearly demonstrated the selectivity brought by the MIP to the determination of LSD in urine. LSD was easily detected in urine at only 0.5 ng/mL with 83% of extraction recovery on the MIP and 11% on the NIP. An LOQ of 0.2 pg/mL was estimated in urine samples.
首次通过非共价印迹方法合成了分子印迹聚合物(MIP),用于从毛发和尿液样本中选择性提取非法药物麦角酸二乙酰胺(LSD)。在MIP的合成中,LSD的类似物用作虚拟模板,甲基丙烯酸用作功能单体,乙腈用作致孔剂溶剂。该MIP用于HPLC-MS分析前的离线萃取。通过研究LSD与MIP之间发生的相互作用,在有机介质中建立了一种选择性方法并应用于毛发样本。通过这种方式,在毛发中成功检测到0.1 ng/mg的LSD,萃取回收率为82%。在对照聚合物上也获得了较低的保留率(仅9%)。然后对该方法进行修改,以在水性介质中进行选择性萃取,用于测定尿液样本中的LSD。与传统C18的比较清楚地证明了MIP在尿液中LSD测定中带来的选择性。在尿液中仅0.5 ng/mL时即可轻松检测到LSD,在MIP上的萃取回收率为83%,在非印迹聚合物(NIP)上为11%。估计尿液样本中的定量限为0.2 pg/mL。