劉 丹,劉濟(jì)寧,吳晟旻,吉貴祥,張圣虎*,石利利*

(1.環(huán)境保護(hù)部南京環(huán)境科學(xué)研究所,江蘇 南京 210042；2.南京工業(yè)大學(xué)化學(xué)與分子工程學(xué)院,江蘇 南京 211816)

太湖水體中對硝基苯酚的分布特征及風(fēng)險(xiǎn)評價(jià)

劉 丹1,2,劉濟(jì)寧1,吳晟旻1,吉貴祥1,張圣虎1*,石利利1*

(1.環(huán)境保護(hù)部南京環(huán)境科學(xué)研究所,江蘇 南京 210042；2.南京工業(yè)大學(xué)化學(xué)與分子工程學(xué)院,江蘇 南京 211816)

為揭示對硝基苯酚(PNP)在太湖及入湖支流水體的污染現(xiàn)狀,通過采集該地區(qū)流域內(nèi)27個(gè)采樣點(diǎn)樣品,采用高效液相色譜質(zhì)譜法(HPLC-MS/MS)對表層水、懸浮顆粒物(SPM)和沉積物中PNP進(jìn)行分析.結(jié)果表明,太湖及入湖支流表層水、SPM和沉積物中PNP的含量分別為12.11～170.20ng/L、115.74～3756.87ng/g和未檢出(ND)～2.65ng/g.入湖支流中的PNP主要分配在表層水中,而SPM中PNP質(zhì)量分?jǐn)?shù)較高的分布于太湖采樣點(diǎn)S16～S21.通過測定沉積物中總有機(jī)碳(TOC),發(fā)現(xiàn)沉積物中PNP的含量與有機(jī)碳的含量有顯著的正相關(guān)性.結(jié)合商值法對PNP的生態(tài)風(fēng)險(xiǎn)進(jìn)行初步評估,結(jié)果表明太湖及其入湖支流中PNP對底棲生物可能存在低生態(tài)風(fēng)險(xiǎn).

對硝基苯酚；風(fēng)險(xiǎn)評價(jià)；太湖

對硝基苯酚(p-nitrophenol,PNP)作為一種重要的單硝基芳香族化合物,大量用作農(nóng)藥、醫(yī)藥、染料等精細(xì)化學(xué)品的中間體,也可用作皮革防霉劑以及酸值指示劑[1-5].由于PNP在生產(chǎn)和使用過程中可以隨生活污水及工業(yè)廢水排放,但是由于污水處理工藝對PNP去除效率較低,大量未被去除的PNP隨出水排放進(jìn)入周圍水環(huán)境,對水生生物和人體健康造成潛在的危害[6-10].生物毒性研究表明PNP是一種具有富集效應(yīng)的危險(xiǎn)物質(zhì),可以通過呼吸和消化系統(tǒng)以及皮膚吸收進(jìn)入生物體,破壞DNA或者抑制DNA的合成,嚴(yán)重影響生物體的血液、肝臟和中樞神經(jīng)系統(tǒng)[11-15].目前研究還發(fā)現(xiàn)PNP可以與雌激素受體和雄激素受體作用表現(xiàn)出雌激素和抗雄激素活性[16-19],此外,體內(nèi)研究表明PNP可以顯著增加未成年雌性小鼠的子宮重量,同時(shí)降低未成年雄性小鼠的附屬性腺重量[20].美國環(huán)保署(EPA)已將PNP列為優(yōu)先控制污染物之一,同時(shí)也將其作為一種潛在的環(huán)境內(nèi)分泌干擾物,規(guī)定在自然水體中的濃度限制在10ng/L以下[21],我國目前也已將PNP列入68種水中優(yōu)先控制污染物黑名單[22].因此,研究水體中PNP的殘留分布情況對了解水體污染狀況以及PNP在水體中行為具有重要意義.

太湖(30°55'N～31°32'N;119°52'E～120°36'E)面積2338km2,平均水深1.9m,是我國第2大淡水湖,位于江蘇省南部,毗鄰常州、無錫、蘇州和湖州[23].太湖不僅具有灌溉、航運(yùn)、水產(chǎn)養(yǎng)殖等功能,同時(shí)也是周邊城市的主要飲用水源[24].由于太湖周邊城市存在有化工廠、印染廠等,可能是PNP的潛在排放源,而目前對于太湖水體中PNP的含量水平和污染特征鮮有報(bào)道[25-26].因此,本研究以太湖及其入湖支流的表層水、懸浮顆粒物和沉積物為研究對象,分析PNP的含量水平,探討暴露濃度與環(huán)境特性之間的關(guān)系,運(yùn)用風(fēng)險(xiǎn)商值法進(jìn)行初步評估,為太湖地區(qū)水環(huán)境中PNP的生態(tài)風(fēng)險(xiǎn)控制和水環(huán)境質(zhì)量管理提供科學(xué)依據(jù).

1 材料與方法

1.1 樣品采集

圖1 太湖及支流采樣分布Fig.1 Sampling sites in Taihu Lake and its tributaries

2015年11月,在太湖及其入湖支流設(shè)置27個(gè)采樣點(diǎn),如圖1所示.使用有機(jī)玻璃采水器采集2L表層水樣(0～1m),裝入棕色玻璃瓶中運(yùn)回實(shí)驗(yàn)室,水樣立即經(jīng)玻璃纖維濾膜(0.45μm) 過濾,過濾后的水樣保存在4℃冰箱內(nèi)待測,同時(shí)將收集到的SPM冷凍干燥,研磨過60目篩,低溫保存待測[27].使用彼得森采泥器采集表層沉積物(0～0.1m),置于不銹鋼盒中,冷凍干燥,研磨過60目篩,低溫保存待測.采用便攜式水質(zhì)監(jiān)測儀現(xiàn)場測定表層水體pH值、溫度和溶解氧(DO).

1.2 儀器與試劑

高效液相色譜-串聯(lián)質(zhì)譜儀(LC-Agilent Technologies 1290Infinity,MS-AB SCIEX QTRAP 4500,美國AB公司);ZORBAX Eclipse Plus C18色譜柱(150mm×2.1mm,3.5μm)(美國Agilent公司);HLB固相萃取小柱(200mg, 6mL)(美國Waters公司);旋轉(zhuǎn)蒸發(fā)儀(瑞士BUCHI公司);Milli-Q超純水器(美國Mimpore公司);AG-285電子天平(瑞士Mettler公司);TOC分析儀(德國Elementar公司).

4-硝基苯酚(4-Nitroaniline,純度99%)購自百靈威科技有限公司;乙腈、甲醇、正己烷(色譜純,德國Merck公司);二氯甲烷(色譜純,美國TEDIA公司);氨水(色譜純,國藥集團(tuán)藥業(yè)股份有限公司);超純水為Milli-Q純水機(jī)出水.

1.3 樣品前處理

水樣:分別用5mL甲醇、5mL超純水活化Oasis HLB(500mg,6mL) 固相萃取小柱,準(zhǔn)確量取經(jīng)0.45μm玻璃纖維濾膜過濾的水樣1L,經(jīng)活化的固相萃取小柱萃取,上樣速度約為5mL/min.上樣后,用10mL的超純水淋洗HLB小柱,并在負(fù)壓條件下抽真空30min進(jìn)行干燥,用10mL甲醇洗脫,洗脫液經(jīng)氮?dú)獯蹈?然后用甲醇/水(v/v= 1/1)定容至1mL,渦旋震蕩2～3min, HPLC-MS/ MS分析.

SPM/沉積物:取1L過濾水樣的SPM和5g沉積物于250mL聚四氟乙烯離心管中,加入50mL二氯甲烷/正己烷(v/v =4/1)混合萃取劑,超聲萃取20min后,以10000r/min離心5min,取上清液,旋轉(zhuǎn)蒸發(fā)至干,用甲醇定容至1.0mL,加入99mL超純水定容,重復(fù)上述水樣處理過程.

1.4 儀器條件

1.4.1 液相色譜 條件采用ZORBAX EclipsePlus C18色譜柱(150mm×2.1mm,3.5μm),流動(dòng)相為0.02%氨水/水(V/V)-乙腈(99:1);流速0.5mL/ min;柱溫40,℃進(jìn)樣5μL.

1.4.2 質(zhì)譜條件 采用電噴霧(ESI)離子源,負(fù)電離模式,多反應(yīng)離子監(jiān)測(MRM)掃描定量分析目標(biāo)污染物.氣簾氣(CUR)壓力為241318Pa,噴霧氣(GS1)壓力為379214Pa,輔助加熱氣(GS2)壓力為413688Pa,源溫度(TEM)為450℃,離子化電壓(IS)為5500V,碰撞氣(CAD),碰撞能量(CE)、去簇電壓(DP)、入口電壓(EP)和出口電壓(CXP)分別為-23,-76,-10,-10V,PNP的母離子與定量子離子(m/z)為138和107.8.

1.5 質(zhì)量保證和質(zhì)量控制(QA/QC)

整個(gè)分析過程按照方法空白、加標(biāo)空白、樣品平行樣進(jìn)行質(zhì)量控制和質(zhì)量保證.在水樣和沉積物空白樣品中進(jìn)行PNP加標(biāo)回收,回收率分別為89.2%～102.3%和78.9%～91.5%,相對標(biāo)準(zhǔn)偏差分別為2.3%～5.8%和1.5%～4.9%,方法空白和加標(biāo)空白均未檢出.

1.6 風(fēng)險(xiǎn)評價(jià)方法

根據(jù)歐盟關(guān)于環(huán)境風(fēng)險(xiǎn)評價(jià)的技術(shù)指導(dǎo),采用風(fēng)險(xiǎn)商值法(RQ)評估太湖水體的環(huán)境風(fēng)險(xiǎn).風(fēng)險(xiǎn)商值(RQ)的計(jì)算公式如下,即實(shí)際測定濃度(MEC)和無效應(yīng)濃度(PNEC)之間的比值[28-29],

PNEC值采用物種敏感度分布法(SSD s)擬合急性/慢性毒性數(shù)據(jù)獲取3個(gè)5%物種危害濃度(即保護(hù)95%物種的污染物濃度),即HC5,急性、HC5,慢性致死和HC5,慢性非致死,并根據(jù)評估因子法選擇相應(yīng)的評估因子(assessment factors, AF),即對于具備3個(gè)營養(yǎng)級物種長期試驗(yàn)數(shù)據(jù)的污染物,采用10為評估因子,對于具備3個(gè)營養(yǎng)級物種短期試驗(yàn)數(shù)據(jù)的污染物,采用1000為評估因子,將HC5除以評估因子,得到PNEC值,具體見文獻(xiàn)[39].根據(jù)RQ值的大小,將環(huán)境風(fēng)險(xiǎn)分為3個(gè)等級,即在0.01～0.1間為低環(huán)境風(fēng)險(xiǎn),在0.1～1.0間為中等環(huán)境風(fēng)險(xiǎn),大于1為高環(huán)境風(fēng)險(xiǎn)[30].由于PNP難以降解,并且可以在有機(jī)質(zhì)介質(zhì)中富集,因此采用平衡分配法計(jì)算太湖表層沉積物中PNP的風(fēng)險(xiǎn)值[31-32].

PNECsed=Kp×PNECwater×1000/RHOSPM(2)式中:PNECsed和PNECwater分別為PNP在沉積物相和水相中的無效應(yīng)濃度, ng/L, ng/g;Kp為SPM-水分配系數(shù),L/L;RHOSPM為SPM的密度, kg/m3.

2 結(jié)果與討論

2.1 水樣中PNP的濃度

圖2 太湖水體中PNP的濃度分布Fig.2 Distribution of PNP in surface water of Taihu Lake

太湖及其入湖支流表層水樣中PNP的濃度分布如圖 2所示.所有采樣點(diǎn)均能檢測到PNP,且支流與太湖水域的污染水平差別較大.表層水中PNP的濃度介于12.11～170.20ng/L,平均值為73.20ng/L.Zhong等[25]于2008年和2009年間采集太湖表層水進(jìn)行分析,未檢測到PNP.與國內(nèi)其它河流相比,本研究中太湖表層水中PNP的殘留量與我國五大流域(黃河、海河、遼河、長江、淮河)24個(gè)典型飲用水源地的殘留量處于同一水平(平均值27.4ng/L)[33],但是遠(yuǎn)低于長江口(表層水樣最大值1.12μg/L)和天津主要污水受納河流(ND～1.77μg/L)[34-35].太湖表層水體中PNP的最高值出現(xiàn)在采樣點(diǎn)(S14),該處靠近宜興工業(yè)園區(qū),工業(yè)園區(qū)地表徑流可能造成該水域PNP含量較高,但是總體空間分布表現(xiàn)為入湖支流(采樣點(diǎn)S4～S10)污染程度較大.太湖入湖支流靠近常州、宜興等工業(yè)城市,工業(yè)污水排放量較大,其中采樣點(diǎn)(S4～S7)處于漕橋河區(qū)域,兩岸約有3000家企業(yè),其中重點(diǎn)控制的污染企業(yè)中化工企業(yè)約占67.7%,印染行業(yè)約占21.2%,采樣點(diǎn)(S8～S10)處于太滆運(yùn)河區(qū)域,周圍61家工業(yè)污染源中以紡織印染企業(yè)為主,其次是化工企業(yè)[36].相較太湖入湖支流及北太湖,其余采樣點(diǎn)表層水中PNP的濃度分布差異不大,這可能是由于南太湖為湖州的水源地,而東太湖為景區(qū)供水水源,水質(zhì)情況相對較好.此外,根據(jù)調(diào)研資料表明,2012年太湖周邊工業(yè)城市生產(chǎn)和使用PNP的用量約為300t/a,在一定程度上表明太湖水體中PNP的污染大部分來自于入湖支流工業(yè)污水的排放.

2.2 SPM中PNP的濃度

太湖及其入湖支流SPM中PNP的濃度分布如圖3所示.在所有采樣點(diǎn)均能檢出PNP,且濃度水平相差很大.SPM中PNP濃度介于115.74～3756.87ng/g,平均值為983.34ng/g.與表層水中PNP濃度分布相比,入湖支流SPM中PNP的濃度相對較低,而采樣點(diǎn)S16～S20含量較高.為評估太湖及其入湖支流表層水與SPM中PNP濃度的相關(guān)性,采用Φ(比例系數(shù))來表征PNP在表層水和SPM間的比例關(guān)系[37]:

式中:CSPM為目標(biāo)化合物在SPM的濃度,ng/g; Cwater為目標(biāo)化合物在水中的濃度,ng/L.

圖3 太湖SPM中PNP的濃度分布Fig.3 Distribution of PNP in SPMof Taihu Lake

PNP在表層水和SPM中的質(zhì)量分?jǐn)?shù)如圖4所示.入湖支流中的PNP主要分配在表層水中,而SPM中PNP質(zhì)量分?jǐn)?shù)較高的采樣點(diǎn)主要位于S16～S21.這可能由于太湖入湖支流水體流速相對較快,而PNP的辛醇-水分配系數(shù)(KOW)并不高(lgKOW=1.91)[38],排放進(jìn)入水體的PNP可能還未與SPM結(jié)合,而采樣點(diǎn)S16～S21水體流速較緩,增加了SPM與表層水中PNP的接觸時(shí)間,使其在水體和SPM中的分配達(dá)到相對穩(wěn)定,此外,雖然采樣點(diǎn)S22～S27的SPM含量相對較高(見表1),但由于表層水中PNP含量相對較低,KOW不高,且可能與SPM自身的有機(jī)物含量,特別是能吸附PNP的物質(zhì)比例小有關(guān),這可能是導(dǎo)致SPM中PNP含量不高的原因.

表1 太湖相關(guān)理化參數(shù)Table 1 Physical and chemical parameters of Taihu Lake

圖4 PNP在水相和SPM之間的比例Fig.4 Proportion of PNP in surface water and SPMphases of Taihu Lake

2.3 沉積物中PNP的濃度

圖5 太湖沉積物中PNP的濃度分布Fig.5 Distribution of PNP in sediment of Taihu Lake

太湖及其入湖支流沉積物中PNP的濃度分布如圖5所示.除了采樣點(diǎn)S3、S7、S26和S27底部為砂石,未采集到沉積物,PNP在其它樣品中的檢出率為91.3%,濃度范圍為ND～2.65ng/g,平均值為1.30ng/g.沉積物中PNP的濃度相較表層水和SPM普遍偏低,可能得益于太湖“清淤工程”的實(shí)施,為太湖水質(zhì)帶來一定程度的改善.由于太湖沉積物中有機(jī)碳(TOC)含量為0.68～5.27%(見表1),平均值1.72%,沉積物中有機(jī)碳含量對其中PNP的含量可能也有著較大影響,因此將沉積物中TOC含量與PNP濃度線性擬合(圖6).由圖6可見,沉積物中PNP的濃度與TOC之間呈現(xiàn)顯著的正相關(guān)(R=0.46,P＜0.05),沉積物中由于富含有機(jī)質(zhì),其復(fù)雜的孔隙結(jié)構(gòu)具有快速吸附污染物的特性,沉積物中TOC含量越高,可吸附的位點(diǎn)越多,越有利于疏水性有機(jī)污染物在表層沉積物中富集.因此沉積物中TOC含量對太湖及其入湖支流PNP的污染水平、歸趨和生物可利用性具有重要影響.

圖6 沉積物中PNP濃度與TOC的相關(guān)性Fig.6 Correlation between the concentration of PNP and TOC in sediment of Taihu Lake

2.4 生態(tài)風(fēng)險(xiǎn)評價(jià)

由于PNP在水生動(dòng)物體內(nèi)的傳遞及富集作用,在一定程度上直接威脅水生生態(tài)系統(tǒng)甚至人體健康,因此對本研究區(qū)域水體中PNP可能對生物造成的生態(tài)風(fēng)險(xiǎn)進(jìn)行評估.采用本課題組近期發(fā)表論文中PNP的PNEC值102μg/L(基于HC5,慢性致死數(shù)據(jù))和47.1μg/L(基于HC5,慢性非致死數(shù)據(jù))[39],根據(jù)PNP在環(huán)境中的MEC,分別計(jì)算PNP基于兩種毒性效應(yīng)終點(diǎn)的生態(tài)風(fēng)險(xiǎn)值RQ慢性致死和RQ慢性非致死,由此計(jì)算得到太湖及其入湖支流水相和沉積物中PNP的風(fēng)險(xiǎn)商值如圖7所示.由圖7可見,表層水中所有采樣點(diǎn)的RQ值(RQ慢性致死和RQ慢性非致死)均小于0.01,即不會(huì)引起生態(tài)風(fēng)險(xiǎn).對于沉積物,PNP的RQ慢性致死值僅在2個(gè)采樣點(diǎn)(S4和S27)大于0.01,而RQ慢性非致死在48%的采樣點(diǎn)均大于0.01,存在低風(fēng)險(xiǎn)危害,這說明PNP對太湖底棲生物生產(chǎn)未造成危害,但是對其繁殖、發(fā)育和生殖可能會(huì)帶來影響.此外,值得關(guān)注的是PNP很難被生物降解且具有蓄積性,會(huì)產(chǎn)生環(huán)境累計(jì)污染,因此對底棲生物的潛在風(fēng)險(xiǎn)不容忽視.

圖7 太湖水相和沉積物相中RQ值Fig.7 RQ values of PNP in water and sediments of Taihu Lake

3 結(jié)論

3.1 太湖及其入湖支流表層水中PNP的含量為12.11～170.20ng/L,SPM和沉積物中PNP的含量分別為115.74～3756.87ng/g 和ND～2.65ng/g.

3.2 在水體-SPM體系中,入湖支流中的PNP主要分配在表層水中,而SPM中PNP質(zhì)量分?jǐn)?shù)較高的采樣點(diǎn)主要位于S16～S21.沉積物中PNP的濃度遠(yuǎn)低于表層水和SPM中的含量,且與沉積物的有機(jī)碳存在顯著的正相關(guān)(R=0.46,P＜0.05).

3.3 用商值法對研究區(qū)域的水體進(jìn)行生態(tài)風(fēng)險(xiǎn)評價(jià)結(jié)果表明,太湖及其入湖支流中PNP對水生生物和底棲生物的生態(tài)風(fēng)險(xiǎn)均在可接受范圍內(nèi),但是由于PNP很難被生物降解且具有蓄積性,會(huì)對環(huán)境產(chǎn)生累計(jì)污染,其潛在危害不容忽視.

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Distribution and ecological risk assessment of p-nitrophenol in Taihu Lake and its tributaries.

LIU Dan1,2, LIU Ji-ning1, WU Sheng-min1, JI Gui-xiang1, ZHANG Sheng-hu1*, SHI Li-li1*
(1.Nanjing Institute of Environmental Sciences, Ministry of Environmental Protection, Nanjing 210042, China；2.College of Chemistry and Molecular Engineering, Nanjing Technglogy University, Nanjing 211816, China). China Environmental Science, 2017,37(2)：761～767

In order to investigate the levels and patterns of PNP in Taihu Lake and its tributaries, 27samples were collected fromthis region and the concentrations of PNP in surface water, suspended particulate matter (SPM) and sediment were determined using high performance liquid chromatography mass spectrometry (HPLC-MS/MS). PNP concentrations in the surface water, SPM and sediment were 12.11～170.20ng/L, 115.74～3756.87ng/g and ND～2.65ng/g, dry weight, respectively. PNP was mainly distributed in surface water in tributaries, while distributed in SPMin sampling site of S16～S21. The total organic carbon (TOC) was also analyzed in this study, and the result indicated that there was obvious positive correlation between the levels of PNP and TOC. In addition, based on the PNP concentration levels, the ecological risks of PNP contamination in Taihu Lake and its tributaries were evaluated by the quotient method. The levels of PNP were considerably lowand this compound may have lowrisk to benthic organisms.

p-nitrophenol；risk assessment；Taihu Lake

X824

A

1000-6923(2017)02-0761-07

劉 丹(1989-),女,江蘇江都人,博士,主要從事化學(xué)品風(fēng)險(xiǎn)暴露和評估工作.發(fā)表論文6篇.

2016-06-20

國家自然科學(xué)基金(21407055);江蘇省自然科學(xué)基金(BK20140115)

* 責(zé)任作者, 張圣虎, 助理研究員, zsh@nies.org; 石利利, 研究員, sll@nies.org