Lagalante Anthony F, Greenbacker Peter W
Villanova University, Department of Chemistry, 800 Lancaster Avenue, Villanova, PA 19085-1699, United States.
Anal Chim Acta. 2007 May 8;590(2):151-8. doi: 10.1016/j.aca.2007.03.027. Epub 2007 Mar 18.
A flow injection analysis (FIA) to quantify imidacloprid was developed based upon (1) ultraviolet (254 nm) photochemical dissociation of imidacloprid to produce nitrite, (2) chemical reduction of the nitrite to nitric oxide by iodide in acid, (3) removal of gas-phase nitric oxide from the aqueous stream using a membrane separator, and (4) detection of the nitric oxide by chemiluminescent reaction with ozone. The cross-reactivity of imidacloprid with eight metabolites of imidacloprid was determined using a commercial ELISA kit and the FIA method. While the ELISA kit demonstrated varying degrees of cross-reactivity, cross-reactivity in the FIA method was observed for only the N-nitro and N-nitroso metabolites. The optimized analytical FIA method, FIA provides a linear response in imidacloprid concentration over four orders of magnitude, has a limit of detection of 5.6 pmol (1.5 ng) of imidacloprid, and exhibits an inter-day precision of 0.4%. Spike-recoveries by FIA demonstrated excellent recovery of imidacloprid in natural waters, hemlock xylem fluid, honey, and grapes with little to no interference from the matrix.
基于以下步骤开发了一种用于定量吡虫啉的流动注射分析(FIA)方法:(1)吡虫啉在紫外线(254 nm)作用下发生光化学解离生成亚硝酸盐;(2)在酸性条件下,亚硝酸盐被碘化物化学还原为一氧化氮;(3)使用膜分离器从水流中去除气相一氧化氮;(4)通过与臭氧的化学发光反应检测一氧化氮。使用商用酶联免疫吸附测定(ELISA)试剂盒和FIA方法测定了吡虫啉与吡虫啉八种代谢物的交叉反应性。虽然ELISA试剂盒显示出不同程度的交叉反应性,但在FIA方法中仅观察到N-硝基和N-亚硝基代谢物存在交叉反应性。优化后的分析FIA方法在吡虫啉浓度四个数量级范围内呈线性响应,吡虫啉的检测限为5.6 pmol(1.5 ng),日间精密度为0.4%。FIA加标回收率表明,在天然水、铁杉木质部液、蜂蜜和葡萄中,吡虫啉的回收率极佳,基质干扰很小或无干扰。