气相色谱/负离子化学电离质谱法测定土壤中硫丹及其代谢物

Determination of Endosulfan and Its Metabolite in soil using Gas Chromatography-mass Spectrometry with Negative Ion Chemical Ionization

中文关键词:  α-硫丹  β-硫丹  硫丹硫酸酯  气相色谱/负离子化学电离质谱法  土壤

英文关键词:α-endosulfan  β-endosulfan  endosulfan sulfate  gas chromatography-negative ion chemical ionization mass spectrometry (GC/MS-NCI)  soil

中文摘要:

      采用气相色谱/负离子化学电离质谱法测定土壤中的硫丹及其代谢物。外标法定量，α-硫丹、β-硫丹及硫丹硫酸酯在0.20～10.0 μg/L范围内线性良好，方法检出限分别为0.02、0.02、0.03 μg/Kg，空白加标平行测定的RSD为3.6%～4.3%，土壤样品加标回收率为83.6%～86.4%。本方法定性定量准确，适用于土壤中硫丹的测定。

英文摘要:

      A gas chromatography-negative ion chemical ionization mass spectrometry (GC/MS-NCI) was developed for the rapid determination of endosulfans and its metabolite in soil samples. The soil sample was pretreated with n-hexane and then analyzed by (GC/MS-NCI). External standard calibration was used; the selective ions of endosulfan and endosulfan sulfate were m/z 406, 408，404, 372 and m/z 386, 384, 352 respectively. The detection limit was 0.02-0.03 μg/Kg. The recoveries were in the range of 83.6%～86.4% with the relative standard deviations less than 5%. The method proposed is efficient, accurate and sensitive, which could meet the requirements for determining endosulfans in soil.