自动固相萃取-GC/MS测定水中多环芳烃和有机氯农药

Determination of PAHs and OCPs in Surface Water by Gas Chromatography/Mass Spectrometry with Automatic Solid-phase Extraction

采用自动固相萃取-气相色谱／质谱技术，建立了地表水中痕量多环芳烃和有机氯农药的检测方法。调节水样pH〈2，加入1％甲醇，使用C18固相萃取柱富集，3mL丙酮＋3mL二氯甲烷洗脱后浓缩定容。采用气相色谱／质谱联用的全扫描模式进行分析，选择特征离子定量，方法检出限为0．026-8．772ng／L。加标水平为0．1μg/L时，样品加标回收率在74．8％～109％之间，RSD为0．01％～14．5％。该方法自动化程度高、快速、准确、重复性好，能满足地表水体中持久性有机污染物分析的要求。

To determine trace amount of PAHs and OCPs in surface water a method was developed using gas chromatography/mass spectrometry with automatic solid-phase extraction. The steps elucidated in this paper were to adjust pH of the water sample to pH〈2, and add 1% methanol, then enrich the sample by C18 extraction cartridge; thereafter, PAHs and OCPs absorbed in the cartridge was eluted by 3 mL acetone plus 3 mL dichloromethane; the sample being concentrated, analysis was conducted by gas chromatography/mass spectrometry using the all-scan mode, and selective ion mass was used in quantitative measurement. Results of the experiment were limits of detection ranged from 0.026 to 8.772 ng/L; when average spiked recoveries for the fishery products at the spiked level attained 0.1 μg/L, ranging from 74.8% to 109%, RSD ranged from 0.01% to 14.5%. It was concluded that the method thus set up was rapid, accurate, sensitive and reliable, and could meet the requirement for analyzing persistent organic pollutants in surface water.