分散固相萃取/气相色谱-串联质谱法分析土壤及沉积物样品中的8种紫外线吸收剂
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摘要
建立了分散固相萃取结合气相色谱-串联质谱测定土壤及沉积物中8种紫外线吸收剂的分析方法,并优化了提取溶剂、提取时间及净化吸附剂等参数。5.0 g样品中加入20 mL正己烷-丙酮(体积比4∶1)及1.0 g SCX净化吸附剂后振荡提取30 min,提取液经浓缩后,采用气相色谱-串联质谱法测定,外标法定量。结果表明,8种紫外线吸收剂在2～150μg/mL质量浓度范围内线性良好,相关系数不小于0.994 7,方法检出限为0.077～0.226 ng/g,在3个加标水平下的平均回收率为95.7%～126%,相对标准偏差(n=8)不大于12%。采用该方法对实际土壤及沉积物样品进行检测,发现UV-328检出率最高。该方法简单、定性定量准确、检出限低,适用于不同类型土壤及沉积物样品中紫外线稳定剂的检测。
A method was established for the determination of 8 UV absorbents in soils and sediments by dispersive solid phase extraction combined with gas chromatography-tandem mass spectrometry(GC-MS/MS).5.0 g sample was extracted by mechanical oscillation method for 30 min after addition of 20 mL hexane-acetone(4 ∶1,by volume)and purification with 1.0 g SCX sorbent.After concentration by rotary evaporator,the extract was determined by GC-MS/MS and quantified by external standard method.Parameters such as extraction solvents,extraction times and types of sorbent were optimized.Results showed that there existed good linear relationships for the target compounds in the range of 2-150 μg/L with their correlation coefficients(r~2) not less than 0.994 7.The detection limits of the method were from 0.077 ng/g to 0.226 ng/g.The average recoveries at three spiked levels ranged from 95.7% to 126% with the relative standard deviations(RSD,n=8)not more than 12%.This method was successfully applied in the analysis of UV absorbents in real samples.The results showed that the detection rate for UV-328 was the highest.The method is simple,accurate and sensitive,and is applicable for the determination of UV absorbents in different types of soil and sediment samples.
A method was established for the determination of 8 UV absorbents in soils and sediments by dispersive solid phase extraction combined with gas chromatography-tandem mass spectrometry(GC-MS/MS).5.0 g sample was extracted by mechanical oscillation method for 30 min after addition of 20 mL hexane-acetone(4 ∶1,by volume)and purification with 1.0 g SCX sorbent.After concentration by rotary evaporator,the extract was determined by GC-MS/MS and quantified by external standard method.Parameters such as extraction solvents,extraction times and types of sorbent were optimized.Results showed that there existed good linear relationships for the target compounds in the range of 2-150 μg/L with their correlation coefficients(r~2) not less than 0.994 7.The detection limits of the method were from 0.077 ng/g to 0.226 ng/g.The average recoveries at three spiked levels ranged from 95.7% to 126% with the relative standard deviations(RSD,n=8)not more than 12%.This method was successfully applied in the analysis of UV absorbents in real samples.The results showed that the detection rate for UV-328 was the highest.The method is simple,accurate and sensitive,and is applicable for the determination of UV absorbents in different types of soil and sediment samples.
引文
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[3] Gou X L,Liu W L,Gao X,Zhou M Q,Zhao X Y.J.Chin.Mass Spectrom.Soc.(勾新磊,刘伟丽,高峡,周明强,赵新颖.质谱学报),2016,37(3):255-261.
[4] Sulej A M,Polkowska Z,Astel A,Namiesnik J.Talanta,2013,117:158-167.
[5] Xu L,Zhang Z F,Liu L Y,Song W W,Ma W L,Li Y F.Environ.Chem.(徐蕾,张子峰,刘丽艳,宋维薇,马万里,李一凡.环境化学),2016,35(3):477-490.
[6] Balmer M E,Buser H R,Müller M D,Poiger T.Environ.Sci.Technol.,2005,39(4):953-962.
[7] Ruan T,Liu R Z,Fu Q,Wang T,Wang Y W,Song S J,Wang P,Teng Man,Jiang G B.Environ.Sci.Technol.,2012,46(4):2071-2079.
[8] Nakata H,Murata S,Filatreau J.Environ.Sci.Technol.,2009,43(18):6920-6926.
[9] Gao C J,Liu L Y,Ma W L,Zhu N Z,Jiang L,Li Y F,Kannan K.Environ.Pollut.,2015,203:1-6.
[10] Tsai D Y,Chen C L,Ding W H.Food Chem.,2014,154:211-216.
[11] Langford K H,Reid M J,Fjeld E,Oxnevad S,Thomas K V.Environ.Int.,2015,80:1-7.
[12] Zhang T,Sun H,Qin X,Wu Q,Zhang Y,Ma J,Kannan K.Sci.Total Environ.,2013,461/462:49-55.
[13] Yamano T,Shimizu M,Noda T.J.Health Sci.,2001,47(2):123-128.
[14] Coronado M,Haro H D,Deng X,Rempel M A,Lavado R,Schlenk D.Aquat.Toxicol.,2008,90(3):182-187.
[15] Krause M,Klit A,Blomberg J M,Soeborg T,Frederiksen H,Schlumpf M,Lichtensteiger W,Skakkebaek N E,Drzewiecki K T.Int.J.Androl.,2012,35(3):424-436.
[16] Qu B C,Bian H T,Mao X Q,Li J.Chin.J.Chromatogr.(曲宝成,边海涛,毛希琴,李尽.色谱),2015,3(12):1327-1332.
[17] Choi S S,Jang J H.Polym.Test.,2011,30(6):673-677.
[18] Ou W H,Tang C M,Wang C W,Jin J B,Peng X Z.Chin.J.Anal.Chem.(欧玮辉,唐才明,王春维,金佳滨,彭先芝.分析化学),2015,43(5):734-741.
[19] Liu R,Ruan T,Wang T,Song S,Guo F,Jiang G B.Talanta,2014,120:158-166.
[20] Liu W,Zhang N,Fan S,Li B,Zhao X D,Wu G H,Xue Y,Zhao R.Chin.J.Anal.Chem.(刘伟,张楠,范赛,李兵,赵旭东,吴国华,薛颖,赵榕.分析化学),2014,42(5):706-710.
[21] Liu Y S,Ying G G,Shareef A,Kookana R S.J.Chromatogr.A,2011,1218:5328-5335.
[22] Wang J,Zhang Z H,Liu Y F,Li Q Z,Yu J L,Peng Y,Zheng J G,Li G K.J.Instrum.Anal.(王晶,张子豪,刘莹峰,李全忠,余建龙,彭莹,郑建国,李攻科.分析测试学报),2016,35(11):1505-1512.
[23] Zhang Q,Liu Y,Gu H,Yu X F,Shao C Y.Chin.J.Anal.Lab.(张强,刘艳,顾华,余肖峰,邵超英.分析试验室),2017,36(3):357-361.
[24] EPA 821-R-16-006.Definition and Procedure for the Determination of the Method Detection Limit- Revision 2.US Environmental Protection Agency (EPA).