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固相萃取/气相色谱-质谱法对土壤中有机氯农药的分析及基质效应研究
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作者单位
刘玲玲,孟甜甜,董希良,任伟,张利钧 济南市环境研究院 
基金项目:山东省自然科学基金(ZR2019PD007)
中文摘要:建立了一种固相萃取/气相色谱-质谱法同时测定土壤中23种有机氯农药的方法,并研究了不同基质效应补偿方式。土壤样品经正己烷∶丙酮(体积比1∶1)提取,弗罗里土小柱净化,采用气相色谱-质谱仪检测。结果发现7种有机氯存在中/强程度的基质效应;在10 mL二氯甲烷∶正己烷(体积比1∶9)+10 mL丙酮∶正己烷(体积比1∶9)为固相萃取的洗脱剂,且脉冲压力为275.8 kPa条件下,可将23种有机氯的基质效应均控制在20%以内。23种有机氯农药在04~10 μg·mL-1质量浓度范围内线性良好,相关系数(r2)均不小于0.999 2,检出限为1.0~8.6 μg·kg-1,定量下限为4.0~34.4 μg·kg-1;在20、60、100 μg·kg-1 3个加标水平下空白土壤中的平均回收率为46.3%~127%,相对标准偏差(n=6)为0.68%~15%。采用该方法在某土壤样品中检出α-六六六、γ-六六六、p,p′-DDE、异狄氏剂醛、p,p′-DDT 5种有机氯农药。
中文关键词:土壤  有机氯  净化  进样条件  基质效应
 
Analysis of Organochlorine Pesticides in Soil by GC-MS with Solid Phase Extraction and Their Matrix Effects Study
Abstract:A method of solid phase extraction/gas chromatography-mass spectrometry was developed for the simultaneous determination of 23 organochlorine pesticides in soil.And different matrix effect compensation approaches were studied.Soil samples were extracted with n hexane-acetone(1∶1,by volume),then purified with a florisil column,and finally detected by GC-MS.Medium or strong matrix effects existed in 7 organic chlorines,which was controlled within 20% for all the 23 organochlorines when 10 mL dichloromethane∶n-hexane(1∶9,by volume) and 10 mL acetone∶n hexane(1∶9,by volume) were selected as the eluents of solid phase extraction,and the pulse pressure was set at 275.8 kPa.Results showed that there was a good linear relationship of the method in the concentration range of 04-10 μg·mL-1 with correlation coefficients(r2) no less than 0.999 2.The limits of detection and limits of quantitation were in the ranges of 1.0-8.6 μg·kg-1 and 4.0-34.4 μg·kg-1,respectively.The average recoveries for blank soil at spiked levels of 20,60 and 100 μg·kg-1 ranged from 46.3% to 109%,with relative standard deviations(RSDs,n=6) of 0.68%-15%.Five organochlorine pesticides,including α-BHC,γ-BHC,p,p′-DDE,endrin aldehyde,p,p′-DDT were detected in a soil sample.
Key Words:soil  organochlorine  clean-up  injection condition  matrix effect
引用本文:刘玲玲,孟甜甜,董希良,任伟,张利钧.固相萃取/气相色谱-质谱法对土壤中有机氯农药的分析及基质效应研究[J].分析测试学报,2020,39(5):646-651.
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