de Perre Chloé, Whiting Sara A, Lydy Michael J
Center for Fisheries, Aquaculture, and Aquatic Sciences, and Department of Zoology, Southern Illinois University, 1125 Lincoln Drive, Life Sciences II, Room 173, Mailcode 6511, Carbondale, IL, 62901, USA.
Arch Environ Contam Toxicol. 2015 May;68(4):745-56. doi: 10.1007/s00244-015-0128-9. Epub 2015 Jan 22.
A method was developed for the extraction and analysis of 2 organophosphate, 8 pyrethroid, and 5 neonicotinoid insecticides from the same water sample. A salted liquid-liquid extraction (LLE) was optimized with a solid-phase extraction (SPE) step that separated the organophosphates (OPs) and pyrethroids from the neonicotinoids. Factors that were optimized included volume of solvent and amount of salt used in the LLE, homogenization time for the LLE, and type and volume of eluting solvent used for the SPE. The OPs and pyrethroids were quantified using gas chromatography-mass spectrometry, and the neonicotinoids were quantified using liquid chromatography-diode array detector. Results showed that the optimized method was accurate, precise, reproducible, and robust; recoveries in river water spiked with 100 ng L(-1) of each of the insecticides were all between 86 and 114 % with RSDs between 2 and 8 %. The method was also sensitive with method detection limits ranging from 0.1 to 27.2 ng L(-1) depending on compounds and matrices. The optimized method was thus appropriate for the simultaneous extraction of 15 widely applied insecticides from three different classes and was shown to provide valuable information on their environmental fate from field-collected aqueous samples.
开发了一种从同一水样中提取和分析2种有机磷酸酯、8种拟除虫菊酯和5种新烟碱类杀虫剂的方法。通过固相萃取(SPE)步骤优化了盐析液液萃取(LLE),该步骤将有机磷酸酯(OPs)和拟除虫菊酯与新烟碱类分离。优化的因素包括LLE中使用的溶剂量和盐量、LLE的匀化时间以及SPE中使用的洗脱溶剂的类型和体积。使用气相色谱 - 质谱法对OPs和拟除虫菊酯进行定量,使用液相色谱 - 二极管阵列检测器对新烟碱类进行定量。结果表明,优化后的方法准确、精密、可重现且稳健;在添加了100 ng L⁻¹每种杀虫剂的河水中,回收率均在86%至114%之间,相对标准偏差在2%至8%之间。该方法也很灵敏,方法检测限根据化合物和基质的不同在0.1至27.2 ng L⁻¹之间。因此,优化后的方法适用于同时从三个不同类别中提取15种广泛应用的杀虫剂,并被证明能从现场采集的水样中提供有关它们环境归宿的有价值信息。