重庆主城两江水体与沉积物中邻苯二甲酸酯和多环芳烃污染水平及特征
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摘要
持久性有机污染物(Persistent Organic Pollutants，简称POPs)对人体健康和环境的影响已经引起全球的广泛关注。城市作为人群聚居地区，水体和沉积物中POPs水平的高低直接影响着城市居民的健康，因而深入研究水体和沉积物中POPs污染物的环境行为对城市生态环境有非常重要意义。邻苯二甲酸酯(PAEs)和多环芳烃(PAHs)是两类典型的POPs污染物，部分PAEs和PAHs化合物被美国环保署(USEPA)列为优先控制污染物。论文选择重庆主城长江、嘉陵江为研究区域，以PAEs和PAHs为研究对象，在建立两类POPs污染物分析方法的基础上，探讨了它们在城市水体和沉积物中的残留水平、污染特征及生态风险。
论文的主要研究结论如下：
①通过单因素试验、Box-Behnken设计并结合响应曲面分析，建立了水样中5种PAEs和16种PAHs同时富集的最佳固相萃取条件：不调节pH值的1L水样加入10mL甲醇改性剂，用Supelco-C_(18)固相萃取小柱进行萃取，上样流速为5.7mL/min，3.4mL二氯甲烷/丙酮/正己烷(体积比1:1:1)混合洗脱剂洗脱，洗脱速率1.1mL/min。GC/MS法测定两类目标物的回收率范围为60.9%~94.6%，方法检出限为0.01~0.4μg/L。分析结果表明，本方法可以取代液液萃取法，并且节省了溶剂，简化了实验步骤。采用超声波提取、层析柱净化对沉积物样品进行预处理，正交实验优化了超声条件。在相同电功率输入情况下（250W），沉积物中PAEs的预处理选择单频超声（45kHz）12min，氧化铝柱净化的方式；对于PAHs选用双频组合超声（28kHz/45kHz）60min，硅胶柱净化。GC/MS法测得沉积物中PAEs、PAHs的加标回收率分别为70.6%~95.6%、75.8%~98.7%，方法检出限为0.54~1.35ng/g、0.36~1.53ng/g，与索氏萃取法相当，优于机械振荡提取法。
②重庆主城两江水相、间隙水和沉积物中5种PAEs浓度分别为53.2~10061.3ng/L、916.8~15807.9ng/L和1438.9~5045.9ng/g，邻苯二甲酸二正丁酯(DnBP)和邻苯二甲酸二(2-乙基己基)酯(DEHP)是水体和沉积物中主要污染物；黏土是影响沉积相中PAEs分布的重要因素(R~2=-0.860，p<0.05)，有机质含量对其影响较小；沉积物-间隙水间的lgK_(oc)值与lg_(Ko)w不相关，DnBP在沉积物和间隙水间的分配接近平衡，邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)有由沉积相向间隙水相迁移的趋势，DEHP则由间隙水相向沉积相迁移；与国内外其他地区相比，研究区水体和沉积物中PAEs含量处于中等偏下水平。
③重庆主城两江16种PAHs在水相中浓度为139.4~1538.6ng/L，间隙水中为563.5~3831.4ng/L，沉积物中642.8~4630.3ng/g；沉积物中的粉砂与PAHs总量显著正相关(R~2=0.625~0.667，p<0.05)，粉砂是影响PAHs分布的重要因素；与其他地区相比，研究区PAHs含量处于中等水平；主成分分析主要反映了PAHs在多介质环境中不完全燃烧来源的相对贡献。其中煤炭、油类燃烧排放对水体中PAHs贡献率为67.8%，天然气燃烧及汽油不完全燃烧的贡献率为9.4%，石油挥发和焦炭来源的贡献率为7.0%；沉积物中，煤炭燃烧、油类燃烧及天然气燃烧排放的贡献率为72.4%，石油挥发及焦炭来源的贡献率为16.8%。
④对沉积物进行粒度分级（>150μm、150~96μm、96~63μm、63~47μm、47~25μm和<25μm），PAEs在<96μm的四个粒度组均有明显富集(富集系数为1.35~1.73)，而PAHs在>150μm、47~25μm和150~96μm三个粒径组中存在富集；不同粒度组分中PAEs含量与TOC含量显著负相关（R~2=-0.784，p<0.05），PAHs含量与之正相关（R~2=0.424），黑碳（BC）对两类污染物的影响都较小。
⑤采用安全阈值法和概率曲线分布法分析了水体中4种PAEs的相对生态风险。结果表明水体中DMP、DEP、DnBP、DEHP的安全阈值分别为15413.16、53302.42、22.84、33.82，对水生生物无风险。以5%水生生物物种受影响作为可接受的效应水平终点（HC_5），采用概率曲线分布进行分析，DnBP、DEHP的浓度超过毒性值的风险概率分别为6.010~(-3)、1.110~(-3)，4种PAEs的风险大小依次为：DnBP>DEHP>DMP>DEP，与安全阈值法结果一致。此外，DEHP和DnBP在沉积相中的含量超过了风险评价低值，可能存在着对生物的潜在危害。
⑥对水体中5种PAHs进行概率风险分析，除萘（Nap）外的其他4种PAHs的安全阈值均小于1，说明菲（Phe）、荧蒽（Flu）、芘（Pyr）和苯并[a]芘（Bap）对水生生物存在潜在风险。以HC_5作为水生生物可接受的效应水平终点，概率曲线分析结果表明Phe、Flu、Pyr、Bap超过毒性值的风险概率分别为0.367、0.394、0.958、0.908，危害化合物的影响大小顺序为Pyr>Bap>Flu>Phe>Nap。此外，两江沉积物单一PAHs含量和PAHs总量均未超过ERM值，严重的PAHs生态风险在沉积物中不存在，负面生物毒性效应会偶尔发生，风险主要来源于3环PAHs，以苊(Ace)、芴(Fle)和菲(Phe)为主。
Persistent organic pollutants (POPs) have become widespread pollutants in theenvironment and now represent a global contamination problem. Hazards associatedwith these pollutants are their persistence in the environment, their bioaccumulationpotential in the tissues of animals and humans through the food chain. Phthalate esters(PAEs) and Polycyclic aromatic hydrocarbons (PAHs) are typical POPs substances inthe environment, some of them listed as priority pollutants. Urban are densely populatedareas, residues level of PAEs and PAHs in water body directly affect the health of urbanresidents. So it is great significant to study PAEs and PAHs on urban water body forurban ecological environment. Taking the Yangtze River and Jialing River aroundChongqing’s Urban Areas as a research object, determination of PAEs and PAHs inwater and sediment, multi-media distribution, sources identification and ecological riskassessment have been discussed in this work. The main findings are as following:
①Solid phase extraction method (SPE) for the simultaneously enrichment of5PAEsand16PAHs in water samples was optimized by the combination of single parameterdesign, Box-Behnken design and response surface analysis. Supelco-C_(18)solid phaseextraction column was used for experiment.10mL methanol was added to1Lunbuffered water samples. The column was rinsed with3.4mL eluting solvent (mixeddichloromethane, acetone and n-hexane with a volume ratio of1:1:1) with a upflowmode at5.7mL/min. The eluting rate was1.1mL/min. In addition, the sediment sampleswere firstly extracted by organic solution, and then PAEs and PAHs sediments sampleswere purified by aluminum oxide chromatography and silica gel chromatographycolumns, respectively. Both PAEs and PAHs were detected by gas chromatography-Mass Spectrometry (GC/MS). Ultrasonic extraction conditions were optimized using anorthogonal array design. The results indicated that under the same ultrasonic power of250W, the best extraction conditions for PAEs was ultrasonicated with a frequency of45kHz for12min and for PAHs was dual-frequency (28kHz/45kHz) for60min. Goodrecoveries rates and limits of quantification of target organic matter in water andsediment were obtained.
②5PAEs were discussed in water phase, pore water and sediment from theYangtze River and Jialing River around Chongqing’s Urban Areas. The total PAEsconcentration ranged from53.2to10061.3ng/L in water phase, from916.8to 15807.9ng/L in pore water and from1438.9to5045.9ng/g in sediment. PAEsconcentration in pore water was much higher than that in the water phase. In fiveanalyzed PAEs compounds, DnBP and DEHP were the main pollutants in water andsediment. Clay content in sediment was the primary factor affecting PAEs distributionwhile organic matter content had less effect in this study. Results of PAEs partitionbetween sediment solid phase and pore water phase showed that there was nocorrelation between lgK_(oc)and lg_(Ko)wof PAEs. When the partitioning of DnBPconcentration between measured sediment and the surrounding pore water tended to beclose to equilibrium, DMP and DEP both had strong trends from sediment to pore waterphase and the opposite tendency was significant for DEHP. As compared to the resultsfor other studies, the PAEs concentration of the study region was in a lower-middlelevel.
③16polycyclic aromatic hydrocarbons (PAHs) were determined in water phase,sediment and pore water in the study areas. Total PAHs concentration ranged from139.4to1538.6ng/L in water phase,563.5to3831.4ng/L in pore water, and642.8to4630.3ng/g in sediment. PAHs concentration had significantly positive correlation withsilt proportion of the sediment (R~2=0.625-0.667，p<0.05), which indicated that siltfraction was a main factor affecting PAHs distribution. Contamination by PAHs inwater and sediment was moderate in comparison with other areas. Sourcesapportionment by principal component analysis reflected PAHs derived fromincompleted combustion. As for dissolved PAHs, coal, oil combustion accounted for67.8%, natural gas and gasoline combustion accounted for9.4%, petroleumvolatilization and coke source accounted for7.0%. As for PAHs in surface sediments,coal, oil and natural gas combustion accounted for72.4%, petroleum volatilization andcoke source accounted for16.8%.
④Sieving was performed to separate the sediments into five sizefractions(>150μm,150-96μm,96-63μm,63-47μm、47-25μm and <25μm). Significantenrichment of PAEs was found in the four franctions of <96μm (enrichment factorswere between1.35and1.73). PAHs were mainly enriched in the fractions of>150μm,47~25μm and150~96μm. PAEs and TOC content showed a linear negative correlation(R~2=-0.784, p<0.05) while PAHs had positive correlation with TOC(R~2=0.424). Blackcarbon (BC) had negeligible influence on the content of PAEs and PAHs.
⑤Based on the observed PAEs concentration in water samplings from the YangtzeRiver and Jialing River around Chongqing’s Urban Areas and NOEC values of aquatic organisms, two probabilistic risk approaches were applied to evaluate ecological risks of4PAEs. It was found that10%of the safety margin value was15413.16,53302.42,22.84and33.82for DMP, DEP, DnBP and DEHP respectively, which indicatednone-potential ecological risk for aquatic organism. In addition, application ofprobability distribution curves in the basic safety margin value and using HC_5(hazardous concentration for5%of species) as the endpoint of effect levels, theprobability of exceeding an exposure concentration for DnBP and DEHP were6.010~(-3)and1.110~(-3)separately. Moreover, associated with this specific probability of effects for4individual PAEs followed the order of DnBP>DEHP>DEP>DMP, which was inaccordance with the method of margin of safety. Surface sediment’s ecological risk instudy area was assessed with the methods of sediment quality guidelines (SQGs).Results showed DEHP and DnBP compound was present in excess of the lower ERLand may exist biological effects.
⑥Probability methodology were adopted to characterize ecological risk of5PAHs in water samples. Safety margin value indicated that Phenanthrene (Phe),Fluoranthene (Flu), Pyrene (Pyr) and Benz[a]pyrene (Bap) had potential ecological riskfor aquatic organism except for Naphthalene (Nap). The harm probabilities of5%of thespecies affected was0.367,0.394,0.958and0.908for Phe, Flu, Pyr and Bap separately,and the risk was in sequence of Pyr>Bap>Flu>Phe>Nap. The result of ecological riskassessment indicated the concentration levels of PAHs in sediment of the study area hadnot caused the marked negative influence on organism. However, Acenaphthene(Ace),Fluorene(Fle) and Phenanthrene compounds were present in excess of the lower ERL,and biological effects might exist. The adverse biological toxicity effect mightoccasionally happen in study areas.
论文的主要研究结论如下：
①通过单因素试验、Box-Behnken设计并结合响应曲面分析，建立了水样中5种PAEs和16种PAHs同时富集的最佳固相萃取条件：不调节pH值的1L水样加入10mL甲醇改性剂，用Supelco-C_(18)固相萃取小柱进行萃取，上样流速为5.7mL/min，3.4mL二氯甲烷/丙酮/正己烷(体积比1:1:1)混合洗脱剂洗脱，洗脱速率1.1mL/min。GC/MS法测定两类目标物的回收率范围为60.9%~94.6%，方法检出限为0.01~0.4μg/L。分析结果表明，本方法可以取代液液萃取法，并且节省了溶剂，简化了实验步骤。采用超声波提取、层析柱净化对沉积物样品进行预处理，正交实验优化了超声条件。在相同电功率输入情况下（250W），沉积物中PAEs的预处理选择单频超声（45kHz）12min，氧化铝柱净化的方式；对于PAHs选用双频组合超声（28kHz/45kHz）60min，硅胶柱净化。GC/MS法测得沉积物中PAEs、PAHs的加标回收率分别为70.6%~95.6%、75.8%~98.7%，方法检出限为0.54~1.35ng/g、0.36~1.53ng/g，与索氏萃取法相当，优于机械振荡提取法。
②重庆主城两江水相、间隙水和沉积物中5种PAEs浓度分别为53.2~10061.3ng/L、916.8~15807.9ng/L和1438.9~5045.9ng/g，邻苯二甲酸二正丁酯(DnBP)和邻苯二甲酸二(2-乙基己基)酯(DEHP)是水体和沉积物中主要污染物；黏土是影响沉积相中PAEs分布的重要因素(R~2=-0.860，p<0.05)，有机质含量对其影响较小；沉积物-间隙水间的lgK_(oc)值与lg_(Ko)w不相关，DnBP在沉积物和间隙水间的分配接近平衡，邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)有由沉积相向间隙水相迁移的趋势，DEHP则由间隙水相向沉积相迁移；与国内外其他地区相比，研究区水体和沉积物中PAEs含量处于中等偏下水平。
③重庆主城两江16种PAHs在水相中浓度为139.4~1538.6ng/L，间隙水中为563.5~3831.4ng/L，沉积物中642.8~4630.3ng/g；沉积物中的粉砂与PAHs总量显著正相关(R~2=0.625~0.667，p<0.05)，粉砂是影响PAHs分布的重要因素；与其他地区相比，研究区PAHs含量处于中等水平；主成分分析主要反映了PAHs在多介质环境中不完全燃烧来源的相对贡献。其中煤炭、油类燃烧排放对水体中PAHs贡献率为67.8%，天然气燃烧及汽油不完全燃烧的贡献率为9.4%，石油挥发和焦炭来源的贡献率为7.0%；沉积物中，煤炭燃烧、油类燃烧及天然气燃烧排放的贡献率为72.4%，石油挥发及焦炭来源的贡献率为16.8%。
④对沉积物进行粒度分级（>150μm、150~96μm、96~63μm、63~47μm、47~25μm和<25μm），PAEs在<96μm的四个粒度组均有明显富集(富集系数为1.35~1.73)，而PAHs在>150μm、47~25μm和150~96μm三个粒径组中存在富集；不同粒度组分中PAEs含量与TOC含量显著负相关（R~2=-0.784，p<0.05），PAHs含量与之正相关（R~2=0.424），黑碳（BC）对两类污染物的影响都较小。
⑤采用安全阈值法和概率曲线分布法分析了水体中4种PAEs的相对生态风险。结果表明水体中DMP、DEP、DnBP、DEHP的安全阈值分别为15413.16、53302.42、22.84、33.82，对水生生物无风险。以5%水生生物物种受影响作为可接受的效应水平终点（HC_5），采用概率曲线分布进行分析，DnBP、DEHP的浓度超过毒性值的风险概率分别为6.010~(-3)、1.110~(-3)，4种PAEs的风险大小依次为：DnBP>DEHP>DMP>DEP，与安全阈值法结果一致。此外，DEHP和DnBP在沉积相中的含量超过了风险评价低值，可能存在着对生物的潜在危害。
⑥对水体中5种PAHs进行概率风险分析，除萘（Nap）外的其他4种PAHs的安全阈值均小于1，说明菲（Phe）、荧蒽（Flu）、芘（Pyr）和苯并[a]芘（Bap）对水生生物存在潜在风险。以HC_5作为水生生物可接受的效应水平终点，概率曲线分析结果表明Phe、Flu、Pyr、Bap超过毒性值的风险概率分别为0.367、0.394、0.958、0.908，危害化合物的影响大小顺序为Pyr>Bap>Flu>Phe>Nap。此外，两江沉积物单一PAHs含量和PAHs总量均未超过ERM值，严重的PAHs生态风险在沉积物中不存在，负面生物毒性效应会偶尔发生，风险主要来源于3环PAHs，以苊(Ace)、芴(Fle)和菲(Phe)为主。
Persistent organic pollutants (POPs) have become widespread pollutants in theenvironment and now represent a global contamination problem. Hazards associatedwith these pollutants are their persistence in the environment, their bioaccumulationpotential in the tissues of animals and humans through the food chain. Phthalate esters(PAEs) and Polycyclic aromatic hydrocarbons (PAHs) are typical POPs substances inthe environment, some of them listed as priority pollutants. Urban are densely populatedareas, residues level of PAEs and PAHs in water body directly affect the health of urbanresidents. So it is great significant to study PAEs and PAHs on urban water body forurban ecological environment. Taking the Yangtze River and Jialing River aroundChongqing’s Urban Areas as a research object, determination of PAEs and PAHs inwater and sediment, multi-media distribution, sources identification and ecological riskassessment have been discussed in this work. The main findings are as following:
①Solid phase extraction method (SPE) for the simultaneously enrichment of5PAEsand16PAHs in water samples was optimized by the combination of single parameterdesign, Box-Behnken design and response surface analysis. Supelco-C_(18)solid phaseextraction column was used for experiment.10mL methanol was added to1Lunbuffered water samples. The column was rinsed with3.4mL eluting solvent (mixeddichloromethane, acetone and n-hexane with a volume ratio of1:1:1) with a upflowmode at5.7mL/min. The eluting rate was1.1mL/min. In addition, the sediment sampleswere firstly extracted by organic solution, and then PAEs and PAHs sediments sampleswere purified by aluminum oxide chromatography and silica gel chromatographycolumns, respectively. Both PAEs and PAHs were detected by gas chromatography-Mass Spectrometry (GC/MS). Ultrasonic extraction conditions were optimized using anorthogonal array design. The results indicated that under the same ultrasonic power of250W, the best extraction conditions for PAEs was ultrasonicated with a frequency of45kHz for12min and for PAHs was dual-frequency (28kHz/45kHz) for60min. Goodrecoveries rates and limits of quantification of target organic matter in water andsediment were obtained.
②5PAEs were discussed in water phase, pore water and sediment from theYangtze River and Jialing River around Chongqing’s Urban Areas. The total PAEsconcentration ranged from53.2to10061.3ng/L in water phase, from916.8to 15807.9ng/L in pore water and from1438.9to5045.9ng/g in sediment. PAEsconcentration in pore water was much higher than that in the water phase. In fiveanalyzed PAEs compounds, DnBP and DEHP were the main pollutants in water andsediment. Clay content in sediment was the primary factor affecting PAEs distributionwhile organic matter content had less effect in this study. Results of PAEs partitionbetween sediment solid phase and pore water phase showed that there was nocorrelation between lgK_(oc)and lg_(Ko)wof PAEs. When the partitioning of DnBPconcentration between measured sediment and the surrounding pore water tended to beclose to equilibrium, DMP and DEP both had strong trends from sediment to pore waterphase and the opposite tendency was significant for DEHP. As compared to the resultsfor other studies, the PAEs concentration of the study region was in a lower-middlelevel.
③16polycyclic aromatic hydrocarbons (PAHs) were determined in water phase,sediment and pore water in the study areas. Total PAHs concentration ranged from139.4to1538.6ng/L in water phase,563.5to3831.4ng/L in pore water, and642.8to4630.3ng/g in sediment. PAHs concentration had significantly positive correlation withsilt proportion of the sediment (R~2=0.625-0.667，p<0.05), which indicated that siltfraction was a main factor affecting PAHs distribution. Contamination by PAHs inwater and sediment was moderate in comparison with other areas. Sourcesapportionment by principal component analysis reflected PAHs derived fromincompleted combustion. As for dissolved PAHs, coal, oil combustion accounted for67.8%, natural gas and gasoline combustion accounted for9.4%, petroleumvolatilization and coke source accounted for7.0%. As for PAHs in surface sediments,coal, oil and natural gas combustion accounted for72.4%, petroleum volatilization andcoke source accounted for16.8%.
④Sieving was performed to separate the sediments into five sizefractions(>150μm,150-96μm,96-63μm,63-47μm、47-25μm and <25μm). Significantenrichment of PAEs was found in the four franctions of <96μm (enrichment factorswere between1.35and1.73). PAHs were mainly enriched in the fractions of>150μm,47~25μm and150~96μm. PAEs and TOC content showed a linear negative correlation(R~2=-0.784, p<0.05) while PAHs had positive correlation with TOC(R~2=0.424). Blackcarbon (BC) had negeligible influence on the content of PAEs and PAHs.
⑤Based on the observed PAEs concentration in water samplings from the YangtzeRiver and Jialing River around Chongqing’s Urban Areas and NOEC values of aquatic organisms, two probabilistic risk approaches were applied to evaluate ecological risks of4PAEs. It was found that10%of the safety margin value was15413.16,53302.42,22.84and33.82for DMP, DEP, DnBP and DEHP respectively, which indicatednone-potential ecological risk for aquatic organism. In addition, application ofprobability distribution curves in the basic safety margin value and using HC_5(hazardous concentration for5%of species) as the endpoint of effect levels, theprobability of exceeding an exposure concentration for DnBP and DEHP were6.010~(-3)and1.110~(-3)separately. Moreover, associated with this specific probability of effects for4individual PAEs followed the order of DnBP>DEHP>DEP>DMP, which was inaccordance with the method of margin of safety. Surface sediment’s ecological risk instudy area was assessed with the methods of sediment quality guidelines (SQGs).Results showed DEHP and DnBP compound was present in excess of the lower ERLand may exist biological effects.
⑥Probability methodology were adopted to characterize ecological risk of5PAHs in water samples. Safety margin value indicated that Phenanthrene (Phe),Fluoranthene (Flu), Pyrene (Pyr) and Benz[a]pyrene (Bap) had potential ecological riskfor aquatic organism except for Naphthalene (Nap). The harm probabilities of5%of thespecies affected was0.367,0.394,0.958and0.908for Phe, Flu, Pyr and Bap separately,and the risk was in sequence of Pyr>Bap>Flu>Phe>Nap. The result of ecological riskassessment indicated the concentration levels of PAHs in sediment of the study area hadnot caused the marked negative influence on organism. However, Acenaphthene(Ace),Fluorene(Fle) and Phenanthrene compounds were present in excess of the lower ERL,and biological effects might exist. The adverse biological toxicity effect mightoccasionally happen in study areas.
引文
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