Le Moullec Sophie, Bégos Arlette, Pichon Valérie, Bellier Bruno
Département Analyse Chimique, Centre d'études du Bouchet, B.P. 3, 91710 Vert-Le-Petit, France.
J Chromatogr A. 2006 Mar 3;1108(1):7-13. doi: 10.1016/j.chroma.2005.12.105. Epub 2006 Jan 31.
The analysis of alkyl alkylphosphonic acids, the degradation products of V and G nerve agents as VX, Sarin or Soman, is an important task for the verification of compliance to the Chemical Weapons Convention. The detection of these contaminants at low concentration levels is often difficult in complex matrices due to the amount of interfering substances. Molecularly imprinted solid-phase extraction technique should allow a selective extraction of these compounds from complex samples, and thus make their detection easier. Two molecularly imprinted polymers (MIPs) prepared with methacrylic acid (MAA) as monomer and pinacolyl methylphosphonic acid (PMPA) as template molecule were synthesised and tested. The first polymer, MIP A, was prepared with ethylene glycol dimethacrylate (EGDMA) in dichloromethane. The second polymer, MIP B, was synthesised using trimethylolpropane trimethacrylate (TRIM) in acetonitrile. To evaluate the selectivity provided by these MIPs, the retention of the ethyl methylphosphonic acid (EMPA) target molecule was studied in parallel on a non-imprinted polymer (NIP). While MIP A does not show any difference compared to NIP A, a good selectivity was obtained for MIP B. After the optimisation of the extraction process, 60% of EMPA can be removed from the NIP B without affecting the retention on the MIP B. A recovery of extraction of 93% was then obtained on the MIP B. Its capacity was then measured and corresponds to 97 microg of EMPA per gram of MIP. Finally, the selectivity of MIP B was clearly demonstrated by applying it to the clean-up of a soil extract spiked with EMPA.
烷基烷基膦酸作为VX、沙林或梭曼等V类和G类神经毒剂的降解产物,其分析对于核查《化学武器公约》的遵守情况而言是一项重要任务。由于干扰物质的存在,在复杂基质中低浓度水平检测这些污染物往往很困难。分子印迹固相萃取技术应能从复杂样品中选择性萃取这些化合物,从而使其检测更容易。合成并测试了两种以甲基丙烯酸(MAA)为单体、频哪基甲基膦酸(PMPA)为模板分子制备的分子印迹聚合物(MIP)。第一种聚合物MIP A是在二氯甲烷中用乙二醇二甲基丙烯酸酯(EGDMA)制备的。第二种聚合物MIP B是在乙腈中用三羟甲基丙烷三甲基丙烯酸酯(TRIM)合成的。为评估这些MIP提供的选择性,同时在非印迹聚合物(NIP)上研究了乙基甲基膦酸(EMPA)目标分子的保留情况。虽然MIP A与NIP A相比没有显示出任何差异,但MIP B获得了良好的选择性。在优化萃取过程后,可从NIP B中去除60%的EMPA,而不影响其在MIP B上的保留。然后在MIP B上获得了93%的萃取回收率。接着测量了其容量,相当于每克MIP吸附97微克EMPA。最后,通过将MIP B应用于加标EMPA的土壤提取物净化,清楚地证明了其选择性。