高效液相色谱法测定土壤和河底泥中的15种邻苯二甲酸酯
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摘要
目的建立土壤和底泥中15种邻苯二甲酸酯的高效液相色谱测定方法,并用于成都市土壤和河底泥中邻苯二甲酸酯(PAEs)的污染调查。方法样品经二氯甲烷提取、离心后,取上清液氮吹至干,乙腈复溶后,进样测定。以Gemini C18(250 mm×4.6 mm,5%μm)为分离柱,乙腈-水为流动相梯度洗脱。结果 DBZP、DIBP、DEHP和DNP的线性范围为0.01～10.0 mg/L,其他PAEs的线性范围为0.005～10.0 mg/L,相关系数均大于0.9998。土壤的检出限(LOD)和定量限(LOQ)分别为1.22～5.56%μg/kg和4.08～18.5%μg/kg,加标回收率和相对标准偏差(RSD)分别为76.4%～111%和1.28%～16.2%;底泥的检出限和定量限分别为0.987～4.35%μg/kg和3.29～14.5%μg/kg,加标回收率和相对标准偏差分别为80.0%～116%和2.11%～11.1%。结论建立的方法具有简便、快速、灵敏、溶剂用量少等优点,适用于土壤和底泥中15种PAEs的同时测定。
Objective The aim of this study was to establish a method for simultaneous determination of 15 phthalates(PAEs)in soil and river by high performance liquid chromatography and apply it to the investigation of PAEs pollution in soil and river sediment in Chengdu, China. Methods PAEs in sample was extracted with dichloromethane, then centrifugated. The supernatant was dried-up under gentle nitrogen flow. Finally, the residue was reconstituted with acetonitrile and the solution was subjected to HPLC analysis. The separation was performed with gradient elution on a Gemini C18 column(250 mm ×4.6 mm, 5μm) and the mobile phase was consisted of acetonitrile and water. Results The linear ranges for DBZP, DIBP,DEHP and DNP were 0.01-10.0 mg/L, and range for the other PAEs were 0.005-10.0 mg/L, with the correlation coefficients greater than 0.9998. The limits of detection(LODs) and the limits of quantification(LOQs) for soil were 1.22-5.56 μg/kg and4.08-18.5 μg/kg, respectively. The recoveries for soil ranged from 76.4% to 111% with RSDs in the range of 1.28%-16.2%.For sediment, the LODs and LOQs were 0.987-4.35 μg/kg and 3.29-14.5 μg/kg, respectively. The recoveries for sediment ranged from 80.0% to 116% with RSDs in the range of 2.11%-11.1%. Conclusion This method is simple, quick, sensitive and solvent-saving. It is suitable for simultaneous determination of 15 PAEs in soil and sediment.
Objective The aim of this study was to establish a method for simultaneous determination of 15 phthalates(PAEs)in soil and river by high performance liquid chromatography and apply it to the investigation of PAEs pollution in soil and river sediment in Chengdu, China. Methods PAEs in sample was extracted with dichloromethane, then centrifugated. The supernatant was dried-up under gentle nitrogen flow. Finally, the residue was reconstituted with acetonitrile and the solution was subjected to HPLC analysis. The separation was performed with gradient elution on a Gemini C18 column(250 mm ×4.6 mm, 5μm) and the mobile phase was consisted of acetonitrile and water. Results The linear ranges for DBZP, DIBP,DEHP and DNP were 0.01-10.0 mg/L, and range for the other PAEs were 0.005-10.0 mg/L, with the correlation coefficients greater than 0.9998. The limits of detection(LODs) and the limits of quantification(LOQs) for soil were 1.22-5.56 μg/kg and4.08-18.5 μg/kg, respectively. The recoveries for soil ranged from 76.4% to 111% with RSDs in the range of 1.28%-16.2%.For sediment, the LODs and LOQs were 0.987-4.35 μg/kg and 3.29-14.5 μg/kg, respectively. The recoveries for sediment ranged from 80.0% to 116% with RSDs in the range of 2.11%-11.1%. Conclusion This method is simple, quick, sensitive and solvent-saving. It is suitable for simultaneous determination of 15 PAEs in soil and sediment.
引文
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[10]李拥军,黎小鹏,李盛安,等.GC-MS法测定底泥中7种邻苯二甲酸酯[J].现代农业科技,2016,(13):221-222.
[11]关卉,王金生,万洪富,等.雷州半岛典型区域土壤邻苯二甲酸酯(PAEs)污染研究[J].农业环境科学学报,2007,26(2):622-628.
[12]Net S,Sempere R,Delmont A,et al.Occurrence,fate,behavior and ecotoxicological state of phthalates in different environmental matrices[J].Environmental Science and Technology,2015,49(7):4019-4035.
[13]林莉,董磊,李青云,等.三峡库区水体和底泥中多环芳烃和邻苯二甲酸酯类分布和来源[J].湖泊科学,2018,30(3):660-667.
[14]Selvaraj KK,Sundaramoorthy G,Ravichandran PK,et al.Phthalate esters in water and sediments of the Kaveri River,India:environmental levels and ecotoxicological evaluations[J].Environmental Geochemistry and Health,2015,37(1):83-96.
[2]成昊,张丽君,张磊,等.基质固相分散萃取-分散液相微萃取-气相色谱/质谱联用法测定土壤中的邻苯二甲酸酯[J].分析试验室,2015,34(5):574-578.
[3]闫蕊,邵明媛,孙长华,等.加速溶剂萃取-高效液相色谱串联质谱法测定土壤中邻苯二甲酸酯[J].分析化学,2014,42(6):897-903.
[4]罗丹玲.城区土壤邻苯二甲酸酯污染特征研究[D].广州:中山大学,2005.
[5]Net S,Delmont A,SempéréR,et al.Reliable quantification of phthalates in environmental matrices(air,water,sludge,sediment and soil):a review[J].The Science of the Total Environment,2015,515-516:162-180.
[6]Hassanzadeh N,Sari AE,Khodabandeh SA.Occurrence and distribution of two phthalate esters in the sediments of the Anzali wetlands on the coast of the Caspian Sea(Iran)[J].Marine Pollution Bulletin,2014,89(1/2):128-135.
[7]Li KK,Ma D,Wu J,et al.Distribution of phthalate esters in agricultural soil with plastic film mulching in Shandong Peninsula,East China[J].Chemosphere,2016,164:314-321.
[8]陈莎,曹莹,苏粤,等.微波萃取气相色谱法测定底泥中邻苯二甲酸酯[J].北京工业大学学报,2009,35(4):498-503.
[9]魏丽琼,呼世斌,刘书慧,等.QuEChERS-高效液相色谱法测定土壤中邻苯二甲酸酯[J].环境工程,2016,34(5):148-151.
[10]李拥军,黎小鹏,李盛安,等.GC-MS法测定底泥中7种邻苯二甲酸酯[J].现代农业科技,2016,(13):221-222.
[11]关卉,王金生,万洪富,等.雷州半岛典型区域土壤邻苯二甲酸酯(PAEs)污染研究[J].农业环境科学学报,2007,26(2):622-628.
[12]Net S,Sempere R,Delmont A,et al.Occurrence,fate,behavior and ecotoxicological state of phthalates in different environmental matrices[J].Environmental Science and Technology,2015,49(7):4019-4035.
[13]林莉,董磊,李青云,等.三峡库区水体和底泥中多环芳烃和邻苯二甲酸酯类分布和来源[J].湖泊科学,2018,30(3):660-667.
[14]Selvaraj KK,Sundaramoorthy G,Ravichandran PK,et al.Phthalate esters in water and sediments of the Kaveri River,India:environmental levels and ecotoxicological evaluations[J].Environmental Geochemistry and Health,2015,37(1):83-96.