Analytical Chemistry Section, CSIR-Indian Institute of Toxicology Research, PO Box 80, M G Marg, Lucknow 226 001, India.
J Chromatogr B Analyt Technol Biomed Life Sci. 2012 May 1;895-896:65-70. doi: 10.1016/j.jchromb.2012.03.015. Epub 2012 Mar 19.
A simple and rapid method to determine the cypermethrin (CYP) insecticide in rat tissues (kidney, liver and brain) and blood has been developed for the first time using low density solvent-dispersive liquid-liquid microextraction (LDS-DLLME) followed by gas chromatography-electron capture detector (GC-ECD) analysis. Initially, tissue samples containing CYP were homoginized in acetone. Subsequently, homogenate was mixed with n-hexane (extraction solvent) and the mixture was rapidly injected into water. The upper n-hexane layer was collected in a separate microtube and injected into GC-ECD for analysis. Blood samples were diluted with ultrapure water and subjected to DLLME through similar procedure. Parameters such as type and volume of disperser and extraction solvent, salting out effect and extraction time, which can affect the extraction efficiency of DLLME, were optimized. Method was validated by investigating linearity, precision, recovery, limit of detection (LOD) and quantification (LOQ). LODs in tissue were in the range of 0.043-0.314 ng mg(-1) and for blood it was 8.6 ng mL(-1) with a signal to noise ratio of 3:1. LOQs in tissue were in the range of 0.143-1.03 ng mg(-1) and for blood it was 28.3 ng mL(-1) with a signal to noise ratio of 10:1. Mean recoveries of CYP at three different concentation levels in all the matrices were found to be in the range of 81.6-103.67%. The results show that, LDS-DLLME coupled with GC-ECD offers a simple, rapid and efficient technique for extraction and determination of CYP in rat tissues and blood samples, which in turn would be useful for toxicological studies of CYP.
首次建立了一种简单、快速的方法,用于检测大鼠组织(肾、肝和脑)和血液中的氯菊酯(CYP)杀虫剂,该方法采用低密度溶剂分散液-液微萃取(LDS-DLLME),随后使用气相色谱-电子捕获检测器(GC-ECD)进行分析。首先,将含有 CYP 的组织样品在丙酮中匀浆。然后,将匀浆与正己烷(萃取溶剂)混合,并迅速将混合物注入水中。上层正己烷层被收集在单独的微管中,并注入 GC-ECD 进行分析。血液样品用超纯水稀释,并通过类似的程序进行 DLLME。优化了分散剂和萃取溶剂的类型和体积、盐析效应和萃取时间等参数,这些参数会影响 DLLME 的萃取效率。通过研究线性、精密度、回收率、检测限(LOD)和定量限(LOQ)对方法进行了验证。组织中的 LOD 范围为 0.043-0.314 ng mg(-1),血液中的 LOD 为 8.6 ng mL(-1),信噪比为 3:1。组织中的 LOQ 范围为 0.143-1.03 ng mg(-1),血液中的 LOQ 为 28.3 ng mL(-1),信噪比为 10:1。在所有基质中,CYP 在三个不同浓度水平的平均回收率均在 81.6-103.67%范围内。结果表明,LDS-DLLME 与 GC-ECD 相结合,为大鼠组织和血液样品中 CYP 的提取和测定提供了一种简单、快速、有效的技术,这对于 CYP 的毒理学研究将是有用的。