Gas Chromatography/Mass Spectrometric Determination of Traces of Hydrophilic and Volatile Organic Compounds in Water after Preconcentration with Activated Carbon
Gas Chromatography/Mass Spectrometric Determination of Traces of Hydrophilic and Volatile Organic Compounds in Water after Preconcentration with Activated Carbon
复制标题
活性炭预浓缩后，气相色谱/质谱法测定水中痕量亲水性和挥发性有机化合物
DOI：
10.2116/analsci.6.843
复制
发表时间：
1990
影响因子：
1.6
通讯作者：
A. Otsuki
中科院分区：
文献类型：
--
作者：
K. Kadokami;Minora Koga;A. Otsuki
作者开发了一种分析方法，用于提取痕量的15种亲水性化合物在水中使用气相色谱/质谱联用活性炭预浓缩程序。作为内标，将全氘代对二氧六环和N，N -二甲基甲酰胺加入到11 μ l水样中，使水通过粒状活性炭柱.用丙酮和二氯甲烷洗脱吸附在活性炭上的有机物质;然后用Kuderna-Danish浓缩器将提取物浓缩至10 ml。采用GC/MS与选择离子监测器（GC/MS-SIM）进行定量分析，以测量15种化合物的回收率加标到水样中的浓度为0。2和2.0 μg/l。除醇类和乙腈外，其余化合物的内标回收率均大于90%，相对标准偏差均小于7%。2微克/升。在本研究中，证实了活性炭预浓缩程序可用于提取log P值（二氯甲烷-水分配系数）大于−0.5的痕量极性化合物，但含有羟基或分子量非常小的化合物除外。该方法已用于河水和海水中极性化合物的分析。检测到对二氧六环、1-丙醇、N -亚硝基二甲胺、N-亚硝基二乙胺、N，N -二甲基甲酰胺和N，N -二甲基乙酰胺低于μg/l水平。
The authors have developed an analytical method for extracting trace amounts of 15 hydrophilic compounds in water using gas chromatography/mass spectrometry coupled with an activated carbon preconcentration procedure. As internal standards, perdeuterated p -dioxane and N,N -imethylformamide were added to 11 of a water sample; the water was passed through a granular activated carbon column. Organic substances adsorbed on the activated carbon were eluted with acetone and dichloromethane; the extract was then concentrated to 10 ml with a Kuderna-Danish concentrator. Quantitative analyses using GC/MS with a selected ion monitor (GC/MS-SIM) were performed to measure the recovery efficiencies of the 15 compounds spiked into water samples at concentrations of 0. 2 and 2.0 μg/l. The recovery efficiencies through the internal standard method of the compounds, except alcohols and acetonitrile, gave more than 90% and their relative standard deviations were less than 7% at a concentration of 0. 2 μg/1. In this study, it was confirmed that the activated carbon preconcentration procedure is useful for extracting trace amounts of polar compounds which have a log P value (dichloromethane-water partition coefficient) greater than −0.5, except for compounds containing a hydroxy group or having a very small molecular weight. The method was applied to the analysis of river water and seawater for polar compounds. p -Dioxane, 1-propanol, N -nitrosodimethylamine, N- nitrosodiethylamine, N,N -dimethylformamide and N,N -dimethylacetamide were detected below the μg/l level.