气相色谱-质谱联用法测定土壤中多类环境内分泌干扰物

Determination of Environmental Endocrine Disrupting Chemicals in Soil by Gas Chromatography-Mass Spectrometry

环境中的内分泌干扰物质种类多样、浓度低且来源广、危害大,对环境中的内分泌干扰物进行及时准确检测,能有效预防环境中的内分泌干扰物造成的危害,是对内分泌干扰物进行预防和治理的关键步骤。因此建立了气相色谱-质谱联用法测定土壤中环境内分泌干扰物(邻苯二甲酸酯类、己二酸酯类、卤代联苯和烷基酚类)含量的方法。样品经丙酮-正己烷(1∶1,V/V)超声提取20min后,采用硅胶固相萃取柱净化,二氯甲烷-丙酮(9∶1,V/V)为洗脱溶剂进行洗脱,在合适的色谱、质谱条件下进行测定。在不同的加标水平下,样品平均加标回收率(n=6)为80.2%～113%,相对标准偏差为2.7%～14.6%,内分泌干扰物定性检测限在0.001～0.013mg/kg,定量检测限在0.003 3～0.042 9mg/kg。方法能很好地应用于土壤中内分泌干扰物高效定量测定。

Endocrine disruptors in the environment are of various types with low concentration, wide source and great harm. Timely and accurate determination of the endocrine disruptors in the environment can effectively prevent the harm, which is a key step for the prevention and treatment of endocrine disrupting chemical in the environment.In this study, the method of gas chromatography-mass spectrometry （GC-MS） for the determination of environmental endocrine disruptors （phthalates, adipates, halogenated biphenyls and alkyl phenols） in soil was established. The samples were ultrasonically extracted by acetone-hexane （1∶1, V/V ） for 20 minutes, purified by silicone solid phase extraction （SPE） column, eluted by dichloromethane-acetone （9∶1, V/V ） and tested under suitable chromatographic mass spectrometry conditions. The average recoveries （ n =6） were 80.2%-113%, and the relative standard deviations were 2.7%-14.6% at different spiked levels. The qualitative detection limit of EDCs was between 0.001-0.013 mg/kg, and the quantitative detection limit was between 0.003 3-0.042 9 mg/kg. The method can be applied to the quantitative analysis of endocrine disruptors in soil.