全自动索氏提取-气相色谱三重四极杆串联质谱法测定土壤中18种多环芳烃
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摘要
建立了全自动索氏提取-气相色谱三重四极杆串联质谱法测定土壤中18种多环芳烃的分析方法。土壤经正己烷和乙酸乙酯(1∶1v/v)提取后,硅胶小柱净化,外标法定量。方法对土壤前处理和仪器条件进行了优化,实际测定结果表明:18种多环芳烃含量在2～50μg/L间呈良好的线性关系,相关系数r2均大于0.997;添加0.05～0.50mg/kg浓度,平均回收率在80.2%～92.4%,相对标准偏差(RSD)为3.2%～8.9%,该方法的灵敏度、准确度和精密度均符合测定的技术要求。
An automatic Soxhlet extraction-gas chromatography triple quadrupole tandem mass spectrometry method for the determination of 18 polycyclic aromatic hydrocarbons(PAHs)in soil was developed.After extraction of hexane and ethyl acetate(1∶1 v/v),the soil was purified by silica gel column and quantified by external standard method.Methods Soil pretreatment and instrumental conditions were optimized.The results showed that 18 PAHs had a good linear relationship between 2-50 g/L,and the correlation coefficient R2 was greater than 0.997.The average recovery was 80.2%-92.4% when 0.05-0.50 mg/kg was added,and RSD was 3.2%-8.9%.The sensitivity and accuracy of the method were satisfactory.And precision meet the technical requirements of the determination.
An automatic Soxhlet extraction-gas chromatography triple quadrupole tandem mass spectrometry method for the determination of 18 polycyclic aromatic hydrocarbons(PAHs)in soil was developed.After extraction of hexane and ethyl acetate(1∶1 v/v),the soil was purified by silica gel column and quantified by external standard method.Methods Soil pretreatment and instrumental conditions were optimized.The results showed that 18 PAHs had a good linear relationship between 2-50 g/L,and the correlation coefficient R2 was greater than 0.997.The average recovery was 80.2%-92.4% when 0.05-0.50 mg/kg was added,and RSD was 3.2%-8.9%.The sensitivity and accuracy of the method were satisfactory.And precision meet the technical requirements of the determination.
引文
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[2]Anderson K A,Szelewski M J,Wilson G,et al.Modified ion sourcetriple quadrupole mass spectrometer gas chromatograph for polycyclicaromatichydrocarbonanalyses[J]. Journalof Chromatography a,2015,1419:89~98.
[3]张玉凤,宋永刚,杨爽,等.气相色谱-三重串联四极杆质谱法测定海洋沉积物中35种多环芳烃[J].海洋环境科学,2017,36(3):468~473.
[4]曹小云,曾楚莹,古文媚,等.气相色谱-三重四极杆串联质谱法测定海产品中18种多环芳烃[J].现代预防医学,2018,45(13):2424~2429.
[5]甘志永,于佩,徐蕾.加速溶剂萃取-GPC净化-GC-MS/MS测定土壤中的16种多环芳烃[J].环境科技,2018,31(2):60~64,69.
[6]石飞云,靳艺,唐宏兵,等.高效液相色谱-二极管阵列检测器串联荧光检测法同时测定空气中的16种多环芳烃[J].中国卫生检验杂志,2017,27(22):3212~3214.
[7]孙红梅,朱玉梅,周军.GC/MS/MS法测定土壤中16种多环芳烃的仪器条件[J].环境与发展,2017,29(7):132~134.
[8]周玮,张盈,秦立新,等.超速匀质超声波辅助萃取-气相色谱/质谱法测定沉积物中多环芳烃[J].化学通报,2017,80(5):460~465.