雄安新区水环境中对羟基苯甲酸酯含量及风险

赵 雪,郑 一,付彩霞,裘文慧,王文科,段 磊,赵 婷

雄安新区水环境中对羟基苯甲酸酯含量及风险

赵 雪1,2,郑 一2*,付彩霞2,裘文慧2,王文科3,段 磊3,赵 婷2

(1.哈尔滨工业大学环境学院,黑龙江 哈尔滨 150090；2.南方科技大学环境科学与工程学院,广东 深圳 518055；3.长安大学环境科学与工程学院,陕西 西安 710054)

于2019年6月对雄安新区和保定市周边地区地表水和地下水进行采样,分析水环境中7种对羟基苯甲酸酯(parabens)组分的含量水平及生态风险.结果表明:对羟基苯甲酸甲酯(MeP)和对羟基苯甲酸丙酯(PrP)的检出率为100%;地表水中的主要组分为MeP,占比达93.4%,地下水中的主要组分为MeP,对羟基苯甲酸乙酯(EtP)和PrP,三者占比达98.0%;地下水中parabens的含量水平高于地表水;地表水中parabens的浓度呈白洋淀下游高于上游的空间分布特征,而地下水中的parabens总量在安新县境内较高,平均浓度可达10.1ng/L;总体而言,当前雄安新区水环境中parabens的污染程度较低、生态风险较小.本文可为未来雄安新区建设中的水环境管理提供污染水平参比值和决策依据,也可为雄安新区水环境中其它药品和个人护理品(PPCPs)的污染研究提供参考.

对羟基苯甲酸酯；药品和个人护理品；雄安新区；地表水；地下水；生态风险；白洋淀

对羟基苯甲酸酯(parabens)是一类被广泛使用的防腐剂,因其具有用量少、成本低、无气味等特点,被广泛添加于食品、药品和化妆品中[1].欧盟、美国食品药品管理局(USFDA)、加拿大卫生部已批准parabens作为食品和化妆品的防腐剂使用,我国的食品添加剂使用卫生标准[GB2760-2007][2]也规定对羟基苯甲酸甲酯(MeP)和丙酯(PrP)可用于食品中.食物、药品和个人护理品(PPCPs)在日常生活及农业畜禽养殖中的应用导致parabens在污水中富集,使其成为水环境中的主要污染来源[3].国内外研究表明,parabens已普遍存在于地表水体,其中MeP、对羟基苯甲酸乙酯(EtP)和PrP是检出率及浓度较高的3种组分,浓度范围在ng/L~μg/L[4-6]之间.地下水中也检出了相应浓度的parabens[7-8].近期研究发现人体血清和尿液中均可检测到parabens[9-10],动物实验结果表明parabens具有雌激素活性[11-13],且其暴露与过敏、哮喘、糖尿病、狼疮以及乳腺癌等免疫相关疾病有关[14-16].因此,parabens类防腐剂的生态风险及其使用安全性已引起了广泛关注.

2017年4月1日,我国正式宣布设立“雄安新区”,旨在建设北京非首都功能集中承载地、京津冀城市群重要一极、高质量高水平社会主义现代化城市.水质安全保障对于雄安新区未来的建设发展至关重要.被誉为“华北明珠”的白洋淀将成为雄安新区的重要水源地之一.由于工业企业和旅游业的发展,以及生活垃圾和生活污水的粗放管理,近年来白洋淀水质恶化[17],重金属[18]、多溴联苯醚[19]、多环芳烃[21]、抗生素[21]等污染物在白洋淀水体中均有检出.总体而言,针对雄安新区水环境中PPCPs类污染物的研究还较为缺乏,而关于地下水环境中parabens的研究尚未见报道.

本研究于2019年6月对雄安新区地表水和地下水进行采样,检测样品中7种parabens组分的浓度,在此基础上分析了地表水和地下水中parabens的污染现状、空间分布特征以及生态风险,以期为未来雄安新区的水环境管理提供污染水平参比值和决策依据,并为当地水环境中其它PPCPs的污染研究提供参考.

1 材料与方法

1.1 研究区域及采样工作

雄安新区位于河北省中部,保定市内,由雄县、安新县和容城县三县及周边区域组成,总面积1566km2,属大清河水系(图1).大清河水系分南北支,上游南支包括萍河、瀑河、漕河、府河、唐河、孝义河和潴龙河等支流,汇入白洋淀西淀;下游北支主要为拒马河,河水由白沟引河入东淀;出淀水经赵王新河进入大清河干流[22].采样时间于2019年6月18 ~ 26日进行,采样点位置如图1所示.地表水样主要采自于白洋淀、入淀河流(南拒马河、白沟引河、瀑河、府河、唐河和孝义河)和大清河干流,共38个采样点,标记为SW1~SW38,其中府河6个(SW1~SW6),瀑河1个(SW7),唐河1个(SW8),孝义河3个(SW9~SW11),白洋淀21个(SW12~ SW32),南拒马河1个(SW33),白沟引河3个(SW34~SW36),大清河干流2个(SW37和SW38).地下水样取自雄安新区三县及保定市周边35口灌溉地下水井,标记UW1~UW35,其中雄县6个(UW1~UW6),容城县5个(UW7~UW11),安新县15个(UW12~UW26),保定市周边地区9个(UW27~ UW35).所采水样置于1L棕色玻璃瓶中,冷藏运至实验室于-4℃冰箱冷藏至样品分析.

图1 研究区域水系及采样点示意

1.2 样品的预处理方法

本研究分析了7种parabens目标物,分别为:对羟基苯甲酸甲酯(MeP)、对羟基苯甲酸乙酯(EtP)、对羟基苯甲酸丙酯(PrP)、对羟基苯甲酸异丙酯(iso-PrP)、对羟基苯甲酸丁酯(BuP)、对羟基苯甲酸异丁酯(iso-BuP)和对羟基苯甲酸苄酯(BzP).

样品处理采用固相萃取法,详细步骤为:取800mL水样过0.45μm滤膜(Millipore),过滤后水相加入50ng13C标记的混合代标(13C-MeP、13C-EtP、13C-PrP、13C-iso-PrP、13C-BuP、13C-iso-BuP和13C-BzP),平衡0.5h.加标后的水样,用隔膜泵抽取上样于经6mL甲醇和6mL超纯水活化后的MCX (6cm3;500mg;Waters)固相萃取柱,流速为1滴/s.上样结束后,固相萃取柱在真空下抽干30min.最后,用14mL甲醇进行洗脱,洗脱液收集于玻璃试管中,氮吹至0.5mL后定容至1mL,转移至2mL棕色色谱瓶中密封低温保存,待上机检测.

1.3 Parabens的仪器分析方法

采用Agilent 公司的液相色谱质谱联用仪(HPLC-MS/MS)对paraben进行定性和定量分析,色谱柱型号为ZORBAX RRHD Eclipse Plus C18(100× 2.1mm,1.8μm).柱温为30℃,流动相为含0.05%甲酸和5mmol/L醋酸铵的超纯水溶液(取5mmol/L, 0.3854g醋酸铵,500μL甲酸溶解在1L超纯水中)和甲醇,梯度洗脱程序如表1所示.质谱选择Dynamic MRM负离子模式,电喷雾电离(ESI),各物质裂解电压、碰撞能量、特征离子对以及保留时间经过优化如表2所示.

1.4 质量控制和质量保证

在样品处理过程中,同时进行2个空白实验和2个基质加标实验,处理方法与水体样品的处理方法相同,用以检测方法回收率和基质干扰.空白样品中parabens的检出浓度远低于其在真实样品中的浓度,本文所报道的浓度数据均已扣除空白值.基质加标样品中7种parabens的回收率范围为89%~135%,表明基质影响较小.另外,为考察方法的回收率,所有样品在处理前均加入7种parabens的代标,其回收率范围为80.6%~103%,表明该方法的回收率较好,本文所报道的浓度数据均经过了代标回收率校正.按照信噪比为10时的标样浓度作为方法定量限,检测方法中目标物的定量限为0.02ng/mL,根据《水环境监测规范》[SL219-2013][23],低于定量限的按照1/2定量限进行计算.

1.5 生态风险评价

地表水和地下水中parabens的潜在生态风险采用风险商(RQ)进行分析,计算公式见式(1)和(2). RQ<0.1表示低风险;0.1£RQ<1表示中度风险;RQ³1表示重度风险[24-25].

RQ=MECW/PNEC(1)

PNEC=LC50/AF(2)

式中: RQ是风险商;MECW是地表水或地下水中parabens的浓度;PNEC是预测无效应浓度;LC50是半致死浓度(即半最大效应浓度),MeP、EtP、PrP、iso-PrP、BuP和BzP的LC50分别是24.6, 18.7, 12.3, 8.5, 5.3和4.0mg/L[25];AF是评价因子,取值为1000.

表1 HPLC梯度洗脱程序

注:流动相A为甲醇,流动相B为超纯水(含0.05%甲酸和0.5%醋酸铵).

表2 Parabens的MRM参数

注: *表示定量离子对.

2 结果与讨论

2.1 地表水中parabens的污染水平及组分构成

本研究区域样品中普遍检出parabens. MeP和PrP在所有地表水样中均有检出(即检出率为100%),而BuP和iso-BuP的检出率较低,分别为7.89%和2.63%.Parabens在地表水样中的浓度和组分构成分别见图2和图3(a).可见, MeP的浓度最高,平均值为2.80ng/L,其次是PrP(0.06ng/L)、iso-PrP (0.05ng/L)、EtP(0.04ng/L)、BzP(0.03ng/L)、BuP (0.01ng/L)和iso-BuP(0.01ng/L).从组成分布来看, MeP是地表水中最主要的成分,占比高达93.4%,这是由于MeP是应用最广泛的一种parabens类防腐剂[26],也间接表明当前城镇化水平很低的雄安新区使用较为单一的parabens类产品.与国内外其它地区地表水研究结果对比发现,雄安新区地表水中MeP (0.92~7.70ng/L)的浓度处于较低水平,远低于北京市内河流(0.81~920ng/L)[27]、湘江(ND~ 3170ng/L)[28]、珠江(ND~1060ng/L)[29]、长江(4.34~ 28.8ng/L)[30]和海河(43.9~241ng/L)[31]等中国境内河流,也低于泰国湄南河(357~2270ng/L)[32]、日本德岛、京都和埼玉县境内河流(ND~525ng/L)[33]、英国塔夫河和伊利河(ND~400ng/L)[34]、瑞士格拉特河(3.10~17.0ng/L)[35]等境外河流.其它几种parabens的污染水平也与MeP类似.综上所述,现阶段雄安新区地表水中parabens的污染水平较低,本研究测得的浓度值可作为未来新区建设发展中parabens污染管控的参比值.

图2 样品中parabens的浓度水平

2.2 地下水中parabens的污染水平及组分构成

MeP、EtP和PrP在地下水样中的检出率为100%,而iso-PrP和iso-BuP的检出率较低,分别为14.3%和22.9%.Parabens在地下水样中的浓度和组成分布分别见图2和图3(b).与地表水不同,地下水中主要组分是MeP、EtP和PrP,分别占总浓度的44.3%、39.1%和14.6%(合计98.0%),平均值分别为3.02,2.66,1.00ng/L,iso-BuP浓度最低,平均值为0.02ng/L.由图3可知,研究区地下水的污染比地表水更为严重(7种parabens在地下水和地表水中的总浓度分别为6.81和3.00ng/L),且parabens的污染来源有所不同(组分构成差异大).可能的原因为:雄县、容城和安新等均以农业生产为主,大量使用农药、化肥并长期进行污水灌溉,加重了地下水的污染负荷[36].国内外针对地下水中parabens的污染研究相对较少,Stuart等[37]报道过英国地下水中MeP和PrP最大可达5000和5500ng/L,Serra-Roig等[7]研究发现西班牙巴塞罗那地下水中MeP和PrP的最大浓度分别为194和61.9ng/L,Peng等[8]发现广州城市垃圾填埋场附近地下水中MeP、PrP和EtP最高可达83.2, 22.5和12.5ng/L,均远高于本研究测得的浓度,可见雄安新区目前地下水的parabens污染程度也相对较低.

图3 样品中parabens的组分构成

2.3 空间分布特征

Parabens浓度在研究区内存在空间差异,如图4所示.在汇入白洋淀的几条地表河流中,∑parabens在大清河干流浓度最高,为6.52ng/L,其次是白洋淀,浓度为3.02ng/L,均高于唐河、府河、孝义河、白沟引河、南拒马河和瀑河等大清河水系上游支流.这些支流因受到沿岸生活污水和工业废水的影响,均受到不同程度的污染[38],这些支流均汇入白洋淀,最终汇入大清河干流,因而导致白洋淀和大清河干流水体中parabens含量升高.白洋淀周围村庄密集,生活污水、垃圾、人畜粪便缺乏有效的收集和处理,其所含的parabens也会以面源形式进入白洋淀.此外,淀内鱼鸭养殖也是可能的污染来源[39].地下水中parabens浓度在安新县高于雄县、保定市周边地区和容城县, ∑parabens的平均浓度分别为10.1, 4.97, 4.90和2.69ng/L.赵本龙等[22]对雄安新区地下水水质调查也发现雄安新区东北部、西北部和靠近白洋淀区域部分水质较差,尤其淀区附近地下水受白洋淀污水影响显著.白洋淀主要位于安新县境内,因此白洋淀水质污染也可能是导致安新县地下水中parabens浓度略高的原因.

图4 不同县区水样中parabens浓度的对比

为样品数量

2.4 生态风险评价

3种主要组分MeP、EtP和PrP在地表水和地下水中的RQ值如图5所示.MeP、EtP和PrP在地表水和地下水中均处于低风险水平(RQ<0.1),这与国内外其它地区的评价结果类似.有研究显示, parabens在中国广东从化流溪河[40]、湖南湘江[28]、印度高韦里河[41]、维拉尔河[41]、西班牙瓜迪亚马尔河[42]等地的地表水中均属低风险水平,而雄安新区地表水中parabens的生态风险比这些地区更低.另一方面,地下水中MeP、EtP和PrP的生态风险均高于地表水,这与前述浓度结果一致,推测是由于当地污水处理设施落后且以农业为主,污水灌溉和畜禽养殖等活动导致地下水中parabens浓度及生态风险升高.位于孝义河入淀口的地下水点位UW15处的风险最高(图5(c)),孝义河是白洋淀4条入淀河流之一,水源主要来自生活污水,保定市印染企业的工业废水也多排入孝义河[43].地下水一旦被污染,其水质恢复的难度大、成本高、时间长.因此,在未来雄安新区的发展建设中,除了完善城市污水处理设施,也应重视周边农村地区污水和垃圾的有效收集和处理,避免地下水parabens污染的生态风险.

3 结论

3.1 雄安新区地表水中可普遍检出7种parabens组分,浓度水平在0.01~2.80ng/L之间,但与国内外其它河流相比,污染程度较轻.MeP为地表水中主要的组分,占比高达93.4%.

3.2 雄安新区地下水中可普遍检出7种常见parabens组分,浓度水平在0.02~3.02ng/L之间,总体上高于当地地表水.MeP、EtP和PrP为主要组分,三者之和占比高达98.0%.

3.3 从浓度的空间分布来看,地表水中parabens浓度呈现白洋淀下游水系高于白洋淀上游水系的特征;对于地下水,安新县的parabens浓度水平较其它地区高,平均浓度可达10.1ng/L.

3.4 雄安新区地表水和地下水中parabens的RQ值均小于1,生态风险较低.

图5 MeP、EtP和PrP在地表水和地下水样品中的RQ值

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Occurrence and ecological risk of parabens in water environment in Xiong’an New Area.

ZHAO Xue1,2, ZHENG Yi2*, FU Cai-xia2, QIU Wen-hui2, WANG Wen-ke3, DUAN Lei3, ZHAO Ting2

(1.School of Environment, Harbin Institute of Technology, Harbin 150090, China；2.School of Environmental Science and Engineering, Southern University of Science and Technology, Shenzhen 518055, China；3.School of Environmental Science and Engineering, Chang’an University, Xi’an 710054, China)., 2021,41(4)：1893~1899

Surface water (SW) and groundwater (GW) samples were taken from Xiong’an New Area and the vicinity of Baoding in June 2019. Concentrations of seven parabens were determined for these samples and the associated ecological risk was assessed. The detection rates of MeP and PrP were 100%. MeP was found to be the predominant compound in SW samples, with a mass contribution of 93.4%, and MeP, EtP and PrP were the predominant compounds in GW samples, with a total mass contribution of 98.0%. The GW samples overall had a higher content of parabens than the SW samples. In space, the SW samples downstream Baiyang Lake showed higher concentrations of parabens than those upstream of Baiyang Lake, while GW samples taken from Anxin County had relatively high concentrations of parabens (10.1ng/L on average). Overall, the water pollution level of parabens, as well as the associated ecological risk, was relatively low in the study area. This study offered reference values for water quality management in the future development of Xiong’an New Area, and sheds light on studies of other PPCPs in the same area.

parabens；PPCPs；Xiong’an New Area；surface water；groundwater；ecological risk；Baiyang Lake

X832

A

1000-6923(2021)04-1893-07

赵 雪(1990-),女,黑龙江鹤岗人,哈尔滨工业大学-南方科技大学联合培养博士生,主要从事新兴污染物在环境中的归趋研究.发表论文9篇.

2020-08-26

国家重点研发计划(2018YFC0406504);国家自然科学基金资助项目(51961125203)

* 责任作者, 教授, zhengy@sustech.edu.cn