Millet M, Wortham H, Sanusi A, Mirabel P
Centre de Géochimie de la Surface (UPR 6251), Université Louis Pasteur, Strasbourg, France.
Arch Environ Contam Toxicol. 1996 Nov;31(4):543-56. doi: 10.1007/BF00212439.
A multiresidue analytical method is described for the analysis of 13 pesticides in fogwater, rainwater, gas, and particles. This method is based upon solid-liquid extraction using Sep-Pak tC18 light cartridges for aqueous samples, soxhlet for gas (adsorbed on XAD-2) and particles (on glass fiber filters), HPLC-based fractionation of the extracted residues using a silica column, and a linear gradient of n-hexane/tert butyl methyl ether followed by GC-ECD and HPLC-UV analyses of each fraction. Prior to analysis with GC-ECD, a methylation procedure using BF3/methanol was developed for the analysis of the fraction which contains chlorophenoxy acid herbicides. The recoveries of the extraction procedure of liquid samples and of the methylation were greater than 92 and 97% with a standard deviation lower than 8 and 5%, respectively. The detection limits varied between 0.1 and 0.01 microgram.ml-1 for the 13 pesticides studied with a standard deviation less than 9%. This method was used for the determination of pesticides in 18 fogwater samples (soluble + insoluble), 31 rainwater samples, and 17 air (gas + particles) samples collected between 1991 and 1993 in Colmar (east of France).
本文描述了一种多残留分析方法,用于分析雾水、雨水、气体和颗粒物中的13种农药。该方法基于以下步骤:对于水样,使用Sep-Pak tC18轻型柱进行固液萃取;对于气体(吸附在XAD-2上)和颗粒物(玻璃纤维滤膜上)进行索氏提取;使用硅胶柱对提取的残留物进行基于高效液相色谱的分级分离;然后用正己烷/叔丁基甲基醚线性梯度洗脱,接着对每个级分进行气相色谱-电子捕获检测(GC-ECD)和高效液相色谱-紫外检测(HPLC-UV)。在用GC-ECD分析之前,开发了一种使用BF3/甲醇的甲基化程序,用于分析含有氯苯氧基酸类除草剂的级分。液体样品萃取程序和甲基化的回收率分别大于92%和97%,标准偏差分别低于8%和5%。所研究的13种农药的检测限在0.1至0.01微克·毫升-1之间,标准偏差小于9%。该方法用于测定1991年至1993年在法国东部科尔马采集的18个雾水样品(可溶+不可溶)、31个雨水样品和17个空气(气体+颗粒物)样品中的农药。