Optimization of pretreatment method for determination of Organophosphate esters in sludge samples
LI Cheng-hui1, ZHU Fen-fen1, QING Da-han2, GAO Xiao-zhong2, HOU Rui2, XU Yi-ping2, WANG Zi-jian1
1. School of Environment and Natural Resources, Renmin University of China, Beijing 100872, China;
2. Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China
In this his study, based on the steps of "enrichment (accelerated solvent extraction) + purification + detection", the operation parameters of sludge sampling volume, extraction conditions, purification column type, wash polarity and eluent polarity were optimized. The optimal parameters include:a sludge sampling volume of 0.2g, an extraction temperature of 130℃, a 1:1 (v/v) solution mixing ratio of acetone/dichloromethane extractant, and an amino column purification operation. A 2:5 (v/v) mixing ratio was used for the dichloromethane/n-hexane wash solution, and dichloromethane was used as the eluent. The qualitative and quantitative detection of organophosphate esters (OPEs) using an ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS) demonstrated:the matrix spike recoveries for all identified OPEs were between 60% and 120% with a matrix effect no more than ±15%. The pretreatment method could also be appropriate for the determination of OPEs in wastewater samples. This pretreatment method was successfully applied to measure the concentrations of OPEs in the water phase and solid phase samples from the main units in a sewage treatment plant in Beijing, and a good result was achieved.
Stevens R, van Es D S, Bezemer R, et al. The structure-activity relationship of fire retardant phosphorus compounds in wood[J]. Polymer Degradation and Stability, 2006,91(4):832-841.
[2]
Kannan S, Kishore K. Absolute Viscosity and Density of Trisubstituted Phosphoric Esters[J]. Journal of Chemical & Engineering Data, 1999,44(4):649-655.
[3]
Official Journal of the European Union. Directive 2003/11/EC of the European Parliament and of the Council of 6February 2003 amending for the 24th time Council Directive 76/769/EEC relating to restrictions on the marketing and use of certain dangerous substances and preparations (pentabromodiphenyl ether, octabromodiphenyl ether)[EB].
[4]
Betts K. Does a key PBDE break down in the environment?[J]. Environmental Science & Technology, 2008,42(18):6781.
[5]
Word Health Organization. Flame retardants:a general introduction[R]. Geneva:WHO, 1997.
[6]
Wei G, Li D, Zhuo M, et al. Organophosphorus flame retardants and plasticizers:Sources, occurrence, toxicity and human exposure[J]. Environmental Pollution, 2015,196:29-46.
[7]
Marklund A, Andersson B, Haglund P. Traffic as a source of organophosphorus flame retardants and plasticizers in snow[J]. Environmental Science & Technology, 2005,39(10):3555-3562.
[8]
Cristale J, Lacorte S. Development and validation of a multiresidue method for the analysis of polybrominated diphenyl ethers, new brominated and organophosphorus flame retardants in sediment, sludge and dust[J]. Journal of Chromatography A, 2013,1305:267-275.
[9]
Norwegian Institute for Water. Research screening of selected metals and new organic contaminants 2007[R]. Norway:NIVA, 2008.
[10]
刘琴,印红玲,李蝶,等.室内灰尘中有机磷酸酯的分布及其健康风险[J]. 中国环境科学, 2017,37(8):2831-2839. LIU Qin, YIN Hong-ling, LI Die, et al. Distribution characteristic of OPEs in indoor dust and its health risk[J]. China Environmental Science, 2017,37(8):2831-2839.
[11]
Word Health Organization. Flame retardants:tris(chloropropyl) phosphate and tris(2-chloroethyl) phosphate[R]. Geneva:WHO, 1998.
[12]
U.S. DOHS. Draft toxicological profile for phosphate ester flame retandants. Georgia:U.S. DOHS, 2009.
[13]
Scientific Committee on Health and Environmental Risks. Risk assessment report on 2,2-bis(chloromethyl)trimethylene bis[bis(2-chloroethyl)phosphate] (V6) environmental part[R]. Brussels:SCHER, 2007.
[14]
Scientific Committee on Health and Environmental Risks. Risk assessment report on TRIS(2-CHLORO-1-METHYLETHYL) PHOSPHATE (TCPP) environmental part[R]. Brussels:SCHER, 2007.
[15]
Scientific Committee on Health and Environmental Risks. Risk assessment report on Tris[2-chloro-1-(chloromethyl) ethyl] phosphate (TDCP) environmental part[R]. Brussels:SCHER, 2007.
[16]
Word Health Organization. Flame retardants:tricresyl phosphate[R]. Geneva:WHO, 1990.
[17]
Fries E, Püttmann W. Occurrence of organophosphate esters in surface water and ground water in Germany[J]. Journal of Environmental Monitoring, 2001,3(6):621-626.
[18]
Bester K. Comparison of TCPP concentrations in sludge and wastewater in a typical German sewage treatment plant-comparison of sewage sludge from 20 plants[J]. Journal of Environmental Monitoring, 2005,7(5):509.
[19]
Quintana J B, Rodil R, Reemtsma T, et al. Organophosphorus flame retardants and plasticizers in water and air Ⅱ. Analytical methodology[J]. TrAC Trends in Analytical Chemistry, 2008,27(10):904-915.
[20]
Marklund A, Andersson B, Haglund P. Screening of organophosphorus compounds and their distribution in various indoor environments[J]. Chemosphere, 2003,53(9):1137-1146.
[21]
Leonards P, Steindal E H, van der Veen I, et al. Screening of organophosphor flame retardants 2010. SPFO-Report 1091/2011. TA-2786/2011.
[22]
Marklund A, Andersson B, Haglund P. Organophosphorus flame retardants and plasticizers in Swedish sewage treatment plants[J]. Environmental Science & Technology, 2005,39(19):7423-7429.
[23]
严小菊.典型OPEs阻燃剂在太湖水体和底泥中存在水平和分布特征[D]. 南京:南京大学, 2013. Yan X. Occurrence and distribution of typical organophorus ester flame retardants in the surface water and sediment in Taihu Lake[D]. Nanjing:Nanjing University, 2013.
[24]
Woudneh M B, Benskin J P, Wang G, et al. Quantitative determination of 13organophosphorous flame retardants and plasticizers in a wastewater treatment system by high performance liquid chromatography tandem mass spectrometry[J]. Journal of Chromatography A, 2015,1400:149-155.
[25]
陈蕾.上海市沉积物中多溴二苯醚和OPEs的污染特征研究[D]. 上海:上海大学, 2015. Chen L. Studies on polybrominated diphenyl ethers and organophosphate esters in sediments of Shanghai[D]. Shanghai:Shanghai University, 2015.
[26]
Brandsma S H, de Boer J, Leonards P E G, et al. Organophosphorus flame-retardant and plasticizer analysis, including recommendations from the first worldwide interlaboratory study[J]. TrAC Trends in Analytical Chemistry, 2013,43:217-228.
[27]
Lu J, Ji W, Ma S, et al. Analysis of organophosphate esters in dust, soil and sediment samples using gas chromatography coupled with mass spectrometry[J]. Chinese Journal of Analytical Chemistry, 2014, 42(6):859-865.
[28]
Zeng X, He L, Cao S, et al. Occurrence and distribution of organophosphate flame retardants/plasticizers in wastewater treatment plant sludges from the Pearl River Delta, China[J]. Environmental Toxicology and Chemistry, 2014,33(8):1720-1725.
[29]
Liang K, Liu J. Understanding the distribution, degradation and fate of organophosphate esters in an advanced municipal sewage treatment plant based on mass flow and mass balance analysis[J]. Science of The Total Environment, 2016,544:262-270.
[30]
庞龙,张肖静,庞榕,等.城市污水处理工艺对OPEs类化合物的去除[J]. 河南师范大学学报(自然科学版), 2016,44(3):98-103. Pang L, Zhang X, Pang R, et al. Removal of organophosphate esters in municipal wastewater treatment process[J]. Journal of Henan Normal University (Natural Science Edition), 2016,44(3):98-103.
[31]
Shi F, Liu J, Liang K, et al. Tris (pentafluoroethyl) trifluorophosphate-based ionic liquids as advantageous solid-phase micro-extraction coatings for the extraction of organophosphate esters in environmental waters[J]. Journal of Chromatography A, 2016,1447:9-16.
[32]
梁钪,牛宇敏,刘景富.超高效液相色谱-串联质谱法测定污水中14种OPEs阻燃剂[J]. 环境化学, 2014,33(10):1681-1685. Liang K, Niu Y, Liu J. Determination of 14organophosphate ester flame retardants in wastewater by UPLC-MS/MS[J]. Environmental Chemistry, 2014,33(10):1681-1685.
