加速溶剂萃取/气相色谱-质谱联用法测定土壤、沉积物和污泥中的10种紫外线吸收剂
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摘要
利用加速溶剂萃取/气相色谱-质谱联用法建立了同时测定土壤、沉积物和污泥中10种紫外线吸收剂的分析方法。样品采用加速溶剂萃取法提取,提取过程中加入硅胶进行同步净化,提取温度为120℃,提取溶剂为甲醇/二氯甲烷混合溶剂(V/V,50/50),静态循环2次,最后采用气相色谱-质谱联用仪分析检测。10种目标化合物的回收率为70.9%~117%,在土壤和沉积物样品中,大部分目标化合物的LOD<1 ng/g,LOQ<4 ng/g;污泥样品中,大部分目标化合物的LOD<10 ng/g,LOQ<30 ng/g,方法灵敏度高,检出限和定量限都较低。应用此方法检测了土壤、沉积物和污泥的实际样品,结果检出了多种紫外线吸收剂,说明紫外线吸收剂在环境中污染问题不容忽视。
A method was developed for simultaneous analysis of 10 typal UV filters in soils, sediments and sludge using accelerated solvent extraction(ASE) and gas chromatography-mass spectrometer(GC-MS). Accelerated solvent extraction was applied as pretreatment methods, with silica gel as an in-cell clean-up sorbent. The extraction solvent was methanol/dichloromethane(V/V, 50∶50), and the extraction temperature 120℃ with 2 cycles. The extraction recoveries of 10 target compounds were range from 70.9% to 117%. The LODs of most targets for soil and sediment samples were lower than 1 ng/g, meanwhile the LOQs were lower than 4 ng/g. For sludge samples, the LODs of most targets were lower than 10 ng/g and the LOQs were lower than 30 ng/g. Several soil, sediment and sludge samples were analyzed with this method, and multiple UV filters were determined. The result showed that the pollution of UV filters was an environmental problem not to be ignored.
A method was developed for simultaneous analysis of 10 typal UV filters in soils, sediments and sludge using accelerated solvent extraction(ASE) and gas chromatography-mass spectrometer(GC-MS). Accelerated solvent extraction was applied as pretreatment methods, with silica gel as an in-cell clean-up sorbent. The extraction solvent was methanol/dichloromethane(V/V, 50∶50), and the extraction temperature 120℃ with 2 cycles. The extraction recoveries of 10 target compounds were range from 70.9% to 117%. The LODs of most targets for soil and sediment samples were lower than 1 ng/g, meanwhile the LOQs were lower than 4 ng/g. For sludge samples, the LODs of most targets were lower than 10 ng/g and the LOQs were lower than 30 ng/g. Several soil, sediment and sludge samples were analyzed with this method, and multiple UV filters were determined. The result showed that the pollution of UV filters was an environmental problem not to be ignored.
引文
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[2]Himmelsbach M,Buchberger W,Reingruber E.Determination of polymer additives by liquid chromatography coupled with mass spectrometry.A comparison of atmospheric pressure photoionization(APPI),atmospheric pressure chemical ionization(APCI),and electrospray ionization(ESI)[J].Polym Degrad Stabil,2009,94:1213-1219.
[3]Kimbrough D R.The photochemistry of sunscreens[J].J Chem Educ,1997,74:51-53.
[4]Kim J-W,Chang K-H,Isobe T,et al.Acute toxicity of benzotriazole ultraviolet stabilizers on freshwater crustacean(Daphnia pulex)[J].Journal of Toxicological Sciences,2011,36:247-251.
[5]Reddy C M,Quinn J G,King J W.Free and bound benzotriazoles in marine and freshwater sediments[J].Environ Sci Technol,2000,34:973-979.
[6]Hartmann P C,Quinn J G,Cairns R W,et al.Depositional history of organic contaminants in Narragansett Bay,Rhode Island,USA[J].Marine Pollution Bulletin,2005,50:388-395.
[7]Nakata H,Murata S,Filatreau J.Occurrence and concentrations of benzotriazole UV stabilizers in marine organisms and sediments from the Ariake Sea,Japan[J].Environ Sci Technol,2009,43:6920-6926.
[8]METI,MHLW,MOE.J-CHECK(Japan CHEmicals Collaborative Knowledge database).Ministry of economy,trade and industry,ministry of health,labour and welfare,and ministry of the environment of Japan.2009.Available online at http://www.safe.nite.go.jp/jcheck/Top.do;jsessionid=E9FD388CF12981F80CEC776C7C897DA1.
[9]Balmer M E,Buser H R,Muller M D,et al.Occurrence of some organic UV filters in wastewater,in surface waters,and in fish from Swiss lakes[J].Environ Sci Technol,2005,39:953-962.
[10]Fent K,Kunz P Y,Zenker A,et al.A tentative environmental risk assessment of the UV-filters3-(4-methylbenzylidene-camphor),2-ethyl-hexyl-4-trimethoxycinnamate,benzophenone-3,benzophenone-4 and 3-benzylidene camphor[J].Marine Environmental Research,2010,69:S4-S6.
[11]Morohoshi K,Yamamoto H,Kamata R,et al.Estrogenic activity of 37 components of commercial sunscreen lotions evaluated by in vitro assays[J].Toxicology in Vitro,2005,19:457-469.
[12]Kunz PY,Fent K.Multiple hormonal activities of UV filters and comparison of in vivo and in vitro estrogenic activity of ethyl-4-aminobenzoate in fish[J].Aquatic Toxicology,2006,79:305-324.