Professional Committee of Rock and Mineral Testing Technology of the Geological Society of China, National Geological Experiment and Testing CenterHost
2020 Vol. 39, No. 4
Article Contents

Ling TONG, Qin TIAN, Zhi-peng YANG, Meng PAN. Research on the Determination of 14 Synthetic Musks in Sediment Samples by Gas Chromatography-Tandem Mass Spectrometry with Accelerated Solvent Extraction[J]. Rock and Mineral Analysis, 2020, 39(4): 587-596. doi: 10.15898/j.cnki.11-2131/td.201906240089
Citation: Ling TONG, Qin TIAN, Zhi-peng YANG, Meng PAN. Research on the Determination of 14 Synthetic Musks in Sediment Samples by Gas Chromatography-Tandem Mass Spectrometry with Accelerated Solvent Extraction[J]. Rock and Mineral Analysis, 2020, 39(4): 587-596. doi: 10.15898/j.cnki.11-2131/td.201906240089

Research on the Determination of 14 Synthetic Musks in Sediment Samples by Gas Chromatography-Tandem Mass Spectrometry with Accelerated Solvent Extraction

  • BACKGROUNDIn recent years, the pollution of synthetic musk in the environment has increased. This kind of material has potential carcinogenic and environmental hormone effects and poses a threat to human health. Therefore, it has attracted increasing attention from scientists. The analytical technology of synthetic musk in environmental samples such as water and soil has developed rapidly. The concentration of synthetic musk in sediments has reached several thousand ng/g, but the methods for the simultaneous extraction and purification and rapid analysis of various types of synthetic musk in complex matrices of sediments are yet to be studied. OBJECTIVESTo establish a rapid method for the analysis of 14 typical synthetic musks in sediment samples by accelerated solvent extraction (ASE) combined with gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS). METHODSAccelerated solvent extraction was used for sample preparation. The ASE cell was filled up with sorbent (0.4g GCB combined with 1.0g SAX) and 5.0g sediment samples. The sample was extracted in two cycles with mixed solvents hexane-acetone (V/V, 4:1) at 80℃. After preconcentration, the extracted solution was determined by GC-MS/MS. RESULTSThe linear range of this method for fourteen target compounds ranged from 5ng/mL to 200ng/mL. The average spike-added recoveries ranged from 70.6% to 121.5%, the relative standard deviations (RSD, n=7) were 0.97%-19.5%. The recoveries of surrogates were 72.2%-116.8%. The detection limits of the method were 0.10-0.19ng/g for nitro musk, 0.09-0.14ng/g for polycyclic musk, and 0.11-1.93ng/g for macrocyclic musk. CONCLUSIONSThis method can satisfy the analysis of musk in sediments with complex matrices.
  • 加载中
  • [1] 曾祥英, 陈多宏, 桂红艳, 等.环境中合成麝香污染物的研究进展[J].环境监测管理与技术, 2006, 18(3):7-10.

    Google Scholar

    Zeng X Y, Chen D H, Gui H Y, et al.Anvance in study on synthetic musk in environment[J].The Admini-stration and Technique of Environmental Monitoring, 2006, 18(3):7-10.

    Google Scholar

    [2] Taylor K M, Weisskopf M, Shine J.Human exposure to nitro musks and the evaluation of their potential toxicity:An overview[J].Environmental Health:A Global Acess Science, 2014, 13:14.

    Google Scholar

    [3] 周启星, 王美娥, 范飞, 等.人工合成麝香的环境污染、生态行为与毒理效应研究进展[J].环境科学学报, 2008, 28(1):1-11.

    Google Scholar

    Zhou Q X, Wang M E, Fan F, et al.Research progress in environmtntal pollution, ecological behavior and toxicological effects of synthetic musks[J].Acta Scientiae Circumstantiae, 2008, 28(1):1-11.

    Google Scholar

    [4] 李菊, 谢建军, 黄雪琳, 等.人造麝香的危害性及其残留检测方法研究进展[J].理化检验(化学分册), 2015, 51(2):272-276.

    Google Scholar

    Li J, Xie J J, Huang X L, et al.Recent advances of researches on the harmfulness of artificial musk and methods of determination of its residual amount[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2015, 51(2):272-276.

    Google Scholar

    [5] 佟玲, 田芹, 潘萌, 等.环境中合成麝香类化合物的残留现状及其分析方法研究进展[J].生态学杂志, 2017, 36(5):1426-1435.

    Google Scholar

    Tong L, Tian Q, Pan M, et al.Recent advances of the research of pollution status and analysis methods for synthetic musks in environment[J].Chinese Journal of Ecology, 2017, 36(5):1426-1435.

    Google Scholar

    [6] Trabalón L, Cano-Sancho G, Pocurull E, et al.Exposure of the population of Catalonia (Spain) to musk fragrances through seafood consumption:Risk assessment[J].Environmental Research:Part B, 2015, 143:116-122.

    Google Scholar

    [7] 王征.气相色谱-负化学源-三重四极杆质谱法测定化妆品中的硝基麝香类化合物[J].色谱, 2012, 30(11):1178-1182.

    Google Scholar

    Wang Z.Determination of synthetic nitro-musks in cosmtics by gas chromatography coupled with negative chemical ionization-triple quadrupole mass spectrometry[J].Chinese Journal of Chromatography, 2012, 30(11):1178-1182.

    Google Scholar

    [8] Ternes T A, Herrmann N, Bonerz M, et al.A rapid method to measure the solid-water distribution coefficient (Kd) for pharmaceuticals and musk fragrances in sewage sludge[J].Water Research, 2004, 38:4075-4084. doi: 10.1016/j.watres.2004.07.015

    CrossRef Google Scholar

    [9] Villa S, Assi L, Ippolito A, et al.First evidences of the occurrence of polycyclic synthetic musk fragrances in surface water systems in Italy:Spatial and temporal trends in the Molgora River (Lombardia Region, Northern Italy)[J].Science of the Total Environment, 2012, 416:137-141. doi: 10.1016/j.scitotenv.2011.11.027

    CrossRef Google Scholar

    [10] Dsikowitzky L, Schwarzbauer J, Littke R.Distribution of polycyclic musks in water and particulate matter of the Lippe River (Germany)[J].Organic Geochemistry, 2002, 33:1747-1758. doi: 10.1016/S0146-6380(02)00115-8

    CrossRef Google Scholar

    [11] Reiner J L, Kannan K.Polycyclic musks in water, sediment, and fishes from the upper Hudson River, New York, USA[J].Water, Air, & Soil Pollution, 2011, 214:335-342.

    Google Scholar

    [12] Hu Z, Shi Y, Cai Y.Concentrations, distribution, and bioaccumulation of synthetic musks in the Haihe River of China[J].Chemosphere, 2011, 84:1630-1635. doi: 10.1016/j.chemosphere.2011.05.013

    CrossRef Google Scholar

    [13] Shek W M, Murphy M B, Lam J C W, et al.Polycyclic musks in green-lipped mussels (Perna viridis) from Hong Kong[J].Marine Pollution Bulletin, 2008, 57:373-380. doi: 10.1016/j.marpolbul.2008.02.037

    CrossRef Google Scholar

    [14] Zhang X, Liang G, Zeng X, et al.Levels of synthetic musk fragrances in human milk from three cities in the Yangtze River Delta in eastern China[J].Journal of Environmental Sciences, 2011, 23:983-990. doi: 10.1016/S1001-0742(10)60506-2

    CrossRef Google Scholar

    [15] Zhang X, Jing Y, Ma L, et al.Occurrence and transport of synthetic musks in paired maternal blood, umbilical cord blood, and breast milk[J].International Journal of Hygiene and Environmental Health, 2015, 218:99-106. doi: 10.1016/j.ijheh.2014.08.005

    CrossRef Google Scholar

    [16] Yin J, Wang H, Zhang J, et al.The occurrence of syn-thetic musks in human breast milk in Sichuan, China[J].Chemosphere, 2012, 87:1018-1023. doi: 10.1016/j.chemosphere.2011.11.068

    CrossRef Google Scholar

    [17] 佟玲, 潘萌, 杨志鹏, 等.搅拌棒萃取-气相色谱-质谱法分析地表水中合成麝香及紫外线吸收剂[J].质谱学报, 2019, 40(3):233-243.

    Google Scholar

    Tong L, Pan M, Yang Z P, et al.Determination of synthetic musks and UV filters in surface water by stir bar sorption extraction and gas chromatography-mass spectrometry[J].Journal of Chinese Mass Spectrometry Society, 2019, 40(3):233-243.

    Google Scholar

    [18] 喻月, 王玲, 赵全升, 等.气相色谱质谱联用测定长江三角洲农田土壤中的合成麝香[J].环境化学, 2015, 34(11):2046-2052.

    Google Scholar

    Yu Y, Wang L, Zhao Q S, et al.Determination of synthetic musks in farmland soil from Yangtze River Delta by gas chromatography-mass spectrometry[J].Environmental Chemistry, 2015, 34(11):2046-2052.

    Google Scholar

    [19] 罗庆, 孙丽娜.微波辅助萃取气相色谱质谱法测定土壤、底泥及植物样品中的多环麝香[J].分析试验室, 2011, 30(4):50-53.

    Google Scholar

    Luo Q, Sun L N.Determination of polycyclic musks in soil, sediment and plants using microwave-assisted solvent extraction with gas chromatography-mass spectrometry[J].Chinese Journal of Analysis Laboratory, 2011, 30(4):50-53.

    Google Scholar

    [20] 胡正君, 史亚利, 蔡亚岐.加速溶剂萃取气相色谱质谱法测定污泥、底泥及土壤样品中的合成麝香[J].分析化学, 2010, 38(6):885-888.

    Google Scholar

    Hu Z J, Shi Y L, Cai Y Q.Determination of synthetic musk fragrances in sewage sludge, sediment and soil using accelerated solvent extraction with gas chromatography-mass spectrometry[J].Chinese Journal of Analytical Chemistry, 2010, 38(6):885-888.

    Google Scholar

    [21] Wang M, Peng C, Chen W, et al.Ecological risks of polycyclic musk in soils irrigated with reclaimed municipal wastewater[J].Ecotoxicology and Environmental Safety, 2013, 97:242-247. doi: 10.1016/j.ecoenv.2013.07.032

    CrossRef Google Scholar

    [22] 丁立平, 郭菁, 陈志涛, 等.分散固相萃取气相色谱质谱联用法测定水产品中的痕量酮麝香[J].色谱, 2013, 31(5):485-489.

    Google Scholar

    Ding L P, Guo J, Chen Z T, et al.Determination of musk ketone in aquatic products by gas chromatography-mass spectrometry with dispersive solid phase extraction[J].Chinese Journal of Chromatography, 2013, 31(5):485-489.

    Google Scholar

    [23] 丁立平, 蔡春平, 林永辉, 等.多重吸附同步净化气相色谱质谱联用法测定水产品中痕量的二甲苯麝香和酮麝香[J].色谱, 2014, 32(3):309-313.

    Google Scholar

    Ding L P, Cai C P, Lin Y H, et al.Determination of trace musk xylene and musk ketone in aquatic products by multiple adsorption synchronous purification-gas chromatography-mass spectrometry[J].Chinese Journal of Chromatography, 2014, 32(3):309-313.

    Google Scholar

    [24] Vallecillos L, Pocurull E, Borrull F.Influence of pre-treatment process on matrix effect for the determination of musk fragrances in fish and mussel[J].Talanta, 2015, 134:690-698. doi: 10.1016/j.talanta.2014.12.010

    CrossRef Google Scholar

    [25] Vallecillos L, Pocurull E, Borrull F.A simple and automated method to determine macrocyclic musk fragrances in sewage sludge samples by headspace solid-phase microextraction and gas chromatography-mass spectrometry[J].Journal of Chromatography A, 2013, 1314:38-43. doi: 10.1016/j.chroma.2013.09.033

    CrossRef Google Scholar

    [26] Wu S F, Ding W H.Fast determination of synthetic polycyclic musks in sewage sludge and sediments by microwave-assisted headspace solid-phase microextraction and gas chromatography-mass spectrometry[J].Journal of Chromatography A, 2010, 1217:2776-2781. doi: 10.1016/j.chroma.2010.02.067

    CrossRef Google Scholar

    [27] Llompart M, Garcıa-Jares C, Salgado C, et al.Determination of musk compounds in sewage treatment plant sludge samples by solid-phase microextraction[J].Journal of Chromatography A, 2003, 999:185-193. doi: 10.1016/S0021-9673(03)00449-7

    CrossRef Google Scholar

    [28] Aguirre J, Bizkarguenaga E, Iparraguirre A, et al.Development of stir-bar sorptive extraction thermal desorption gas chromatography-mass spectrometry for the analysis of musks in vegetables and amended soils[J].Analytica Chimica Acta, 2014, 812:74-82. doi: 10.1016/j.aca.2013.12.036

    CrossRef Google Scholar

    [29] Vallecillos L, Pedrouzo M, Pocurull E, et al.Headspace stir bar sorptive extraction followed by thermal desorption and gas chromatography with mass spectrometry to determine musk fragrances in sludge samples without sample pretreatment[J].Journal of Separation Science, 2014, 37:1322-1329. doi: 10.1002/jssc.201400048

    CrossRef Google Scholar

    [30] 李贵梅, 陈东辉, 黄满红, 等.固相萃取-气质联用测定水环境中痕量多环麝香[J].分析试验室, 2011, 30(1):55-58.

    Google Scholar

    Li G M, Chen D H, Huang M H, et al.Study on determination of polycyclic musks in water by GC-MS with solid-phase extraction[J].Chinese Journal of Analysis Laboratory, 2011, 30(1):55-58.

    Google Scholar

    [31] Vallecillos L, Borrull F, Eva P.Determination of musk fragrances in sewage sludge by pressurized liquid extration coupled to automated ionic liquid-based headspace single-drop microextraction followed by GC-MS/MS[J].Journal of Separation Science, 2012, 35:2735-2742. doi: 10.1002/jssc.201200326

    CrossRef Google Scholar

    [32] 吴春英, 白鹭, 陆文龙, 等.气相色谱串联质谱法同时快速检测环境水样中11种合成麝香[J].分析科学学报, 2016, 32(2):188-192.

    Google Scholar

    Wu C Y, Bai L, Lu W L, et al.Simutaneous and rapid determination of 11 synthetic musks in environmental water samples using gas chromatography-tandem mass spectrometry[J].Journal of Analytical Science, 2016, 32(2):188-192.

    Google Scholar

    [33] 佟玲, 杨佳佳, 阎妮, 等.加速溶剂提取/GC-MS对动物组织中有机氯农药和多氯联苯的同时测定[J].岩矿测试, 2014, 33(2):262-269.

    Google Scholar

    Tong L, Yang J J, Yan N, et al.Simultaneous analysis of organochlorinated pesticides and polychlorinated biphenyls from animal tissue using gas chromatography mass spectrometry combined with accelerated solvent extraction[J]. Rock and Mineral Analysis, 2014, 33(2):262-269.

    Google Scholar

    [34] Zhang X, Yao Y, Zeng X, et al.Synthetic musks in the aquatic environment and personal care products in Shanghai, China[J].Chemosphere, 2008, 72:1553-1558. doi: 10.1016/j.chemosphere.2008.04.039

    CrossRef Google Scholar

    [35] 车金水, 虞锐鹏, 王利平, 等.太湖流域人工合成麝香的分布调查研究[J].香料香精化妆品, 2010(6):12-16.

    Google Scholar

    Che J S, Yu R P, Wang L P, et al.Investigation on content of distribution of the synthetic musks in Taihu Lake[J]. Flavour Fragrance Cosmetics, 2010(6):12-16.

    Google Scholar

  • 加载中
通讯作者: 陈斌, bchen63@163.com
  • 1. 

    沈阳化工大学材料科学与工程学院 沈阳 110142

  1. 本站搜索
  2. 百度学术搜索
  3. 万方数据库搜索
  4. CNKI搜索

Figures(3)

Tables(5)

Article Metrics

Article views(4537) PDF downloads(72) Cited by(0)

Access History

Other Articles By Authors

Catalog

    /

    DownLoad:  Full-Size Img  PowerPoint