Kim Kyu Bong, Bartlett Michael G, Anand Sathanandam S, Bruckner James V, Kim Hyo Jung
Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens, 30602, USA.
J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Apr 13;834(1-2):141-8. doi: 10.1016/j.jchromb.2006.02.039. Epub 2006 Mar 22.
Deltamethrin (DLM), [(S)-alpha-cyano-d-phenoxybenzyl-(1R,3R)-e-(2,2 dibromovinyl)-2,2-dimethylcyclo-propane-1-carboxylate], is a pyrethroid insecticide widely used in agriculture and households. There are several methods for analysis of DLM in biological fluids and tissues, but these methods are time consuming. They generally involve the extraction of DLM with lipid-soluble solvents such as n-pentane, n-hexane, diethylether or acetone, and subsequent evaporation of the solvent. A more rapid and sensitive high-performance liquid chromatography (HPLC) method to analyze DLM in plasma and tissues (liver, kidney, and brain) was developed and validated according to U.S. Food and Drug Administration (U.S. FDA) and International Conference on Harmonization (ICH) of Technical Requirements for Registration of Pharmaceuticals for Human Use guidelines. The limit of detection (S/N of 3/1) for DLM was 0.01 microg/ml for plasma, liver, kidney and brain. The method performances were shown to be selective for DLM and linear over the concentration range 0.01-20.0 microg/ml. For five replications of samples at 0.05, 0.1, 0.2, 1.5 and 4.0 microg/ml, intraday precision and accuracy values were in the range of 0.7-13.1% relative standard deviation (%R.S.D.) and 1.8-14.1%Error, respectively. Interday (n = 15) precision and accuracy values at 0.05, 0.1, 0.2, 1.5, and 4.0 microg/ml were in the range of 3.2-15.2% (%R.S.D.) and 3.7-14.8%Error, respectively. The absolute recoveries of DLM ranged from 93 to 103% for plasma, 95 to 114% for liver, 97 to 108% for kidney, and 95 to 108% for brain. This method can be quite useful for DLM pharmacokinetic and tissue distribution studies, for which multiple plasma and tissue samples have to be analyzed quickly with high reproducibility.
溴氰菊酯(DLM),即[(S)-α-氰基-对苯氧基苄基-(1R,3R)-顺式-(2,2-二溴乙烯基)-2,2-二甲基环丙烷-1-羧酸酯],是一种广泛应用于农业和家庭的拟除虫菊酯类杀虫剂。生物体液和组织中DLM的分析方法有多种,但这些方法耗时较长。它们通常涉及用脂溶性溶剂(如正戊烷、正己烷、乙醚或丙酮)提取DLM,随后蒸发溶剂。根据美国食品药品监督管理局(U.S. FDA)和人用药品注册技术要求国际协调会(ICH)的指导原则,开发并验证了一种更快速、灵敏的高效液相色谱(HPLC)法,用于分析血浆和组织(肝脏、肾脏和大脑)中的DLM。血浆、肝脏、肾脏和大脑中DLM的检测限(信噪比为3/1)为0.01μg/ml。该方法对DLM具有选择性,在0.01 - 20.0μg/ml的浓度范围内呈线性。对于0.05、0.1、0.2、1.5和4.0μg/ml的样品进行五次重复分析,日内精密度和准确度值的相对标准偏差(%R.S.D.)范围为0.7 - 13.1%,误差范围为1.8 - 14.1%。在0.05、0.1、0.2、1.5和4.0μg/ml时的日间(n = 15)精密度和准确度值的相对标准偏差(%R.S.D.)范围分别为3.2 - 15.2%和误差范围为3.7 - 14.8%。DLM的绝对回收率在血浆中为93%至103%,在肝脏中为95%至114%,在肾脏中为97%至108%,在大脑中为95%至108%。该方法对于DLM的药代动力学和组织分布研究非常有用,因为在这些研究中需要快速且具有高重现性地分析多个血浆和组织样品。