全血中多种农药在线凝胶渗透色谱净化气相色谱质谱法的快速测定

Rapid determination of 28 pesticides and tetramine in whole blood by online gel permeation chromatography coupled with gas chromatography-mass spectrometry

目的 建立全血中28种农药及鼠药的在线凝胶渗透色谱净化气相色谱-质谱（GPC-GC-MS）快速检测方法.方法 全血样品经乙腈简单提取后,经过在线凝胶渗透色谱（GPC）净化,去除血液中的蛋白、脂肪等大分子物质后,大体积进样到气相色谱质谱（GCMS）进行分析.结果 使用外标法绘制27种农药和1种鼠药的校准曲线,28种样品的0.1-0.5 mg/L浓度范围线性关系良好,相关系数为0.994 9-0.999 9,定量检出限为0.005-0.060 mg/L;全血中28种样品和鼠药在0.1-0.5 mg/L之间,除百菌清回收效率低外,其余样品加标回收率为43.0％-103.2％,大部分样品的相对标准偏差＜10％.结论 该方法简便,快速,准确,灵敏度高,可满足中毒血样中多种农药同时测定的要求.

Objective To study the influences of carbon disulfide （CS2） exposure on fatty acid metabolism in apolipoprotein E （ApoE） knockout mice and C57BL/6J mice.Methods Twenty-four male ApoE knockout mice were randomly and equally divided into four groups：a CS2-exposed normal diet group,a CS2-unexposed normal diet group,a CS2-exposed high-fat diet group,and a CS2-unexposed high-fat diet group.Twenty-four C57BL/6J male mice were divided into four groups in the same way.The CS2-exposed groups were exposed to CS2 （1 g/m^3） by static inhalation for 5 hours a day,5 days a week.After two weeks,the whole blood of mice was collected.Methyl ester derivatization of fatty acids was performed using an acid-catalyzed method.Fatty acid contents before and after exposure were compared by gas chromatography-mass spectroscopy.Results There were significant differences in fatty acid contents of mice between the four groups.For the C57BL/6J mice,the arachidic acid contents in the CS2-exposed high-fat diet group were significantly lower than those in the CS2-unexposed high-fat diet group （P=0.0450）.For the ApoE knockout mice,the arachidonic acid contents in the CS2-exposed normal diet group were significantly lower than those in the CS2-unexposed control diet group （P=0.0452）.For the ApoE knockout mice,the y-linolenic acid contents in the CS2-exposed high-fat diet group were significantly higher than those in the unexposed high-fat diet group （P=0.0447）.Conclusion Exposure to CS2 can induce fatty acid metabolism disorder in mice,indicating that CS2 may increase the risk of atherosclerosis and other cardiovascular diseases.