Catalá-Icardo M, Meseguer-Lloret S, Torres-Cartas S
Instituto de Investigación para la Gestión Integrada de Zonas Costeras. Universitat Politècnica de València, C/Paranimf no 1, 46730 Grao de Gandía, Valencia, Spain.
Photochem Photobiol Sci. 2016 May 11;15(5):626-34. doi: 10.1039/c6pp00056h. Epub 2016 Apr 15.
A liquid chromatography method with post-column photoinduced chemiluminescence (PICL) detection is proposed for the simultaneous determination of eight carbamate pesticides, namely aldicarb, butocarboxim, ethiofencarb, methomyl, methiocarb, thiodicarb, thiofanox and thiophanate-methyl. After chromatographic separation, quinine (sensitizer) was incorporated and the flow passed through an UV lamp (67 s of irradiation time) to obtain the photoproducts, which reacted with acidic Ce(iv) and provided a CL emission. The PICL method showed great selectivity for carbamate pesticides containing sulphur in their chemical structure. A solid-phase extraction process increased sensitivity (LODs ranging from 0.06 to 0.27 ng mL(-1)) and allowed the carbamate pesticides in surface and ground water samples to be determined, with recoveries in the range 87-110% (except for thiophanate-methyl, whose recoveries were between 60 and 75%). The intra- and inter-day precision was evaluated, with RSD ranging from 1.1 to 7.5% and from 2.6 to 12.3%, respectively. A discussion about the PICL mechanism is also included.
提出了一种柱后光致化学发光(PICL)检测的液相色谱法,用于同时测定八种氨基甲酸酯类农药,即涕灭威、丁硫克百威、乙硫苯威、灭多威、甲硫威、硫双威、硫线磷和甲基托布津。色谱分离后,加入奎宁(敏化剂),流动相通过紫外灯(照射时间67秒)以获得光产物,该光产物与酸性Ce(IV)反应并产生化学发光发射。PICL方法对化学结构中含硫的氨基甲酸酯类农药具有很高的选择性。固相萃取过程提高了灵敏度(检测限范围为0.06至0.27 ng mL-1),并能够测定地表水和地下水样品中的氨基甲酸酯类农药,回收率在87-110%范围内(甲基托布津除外,其回收率在60-75%之间)。评估了日内和日间精密度,相对标准偏差分别在1.1至7.5%和2.6至12.3%范围内。还包括对PICL机制的讨论。