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浙江大学学报（农业与生命科学版）
浙江大学学报（农业与生命科学版）  2019, Vol. 45 Issue (3): 365-375    DOI: 10.3785/j.issn.1008-9209.2018.03.282
资源利用与环境保护     
海洋沉积物中邻苯二甲酸酯类环境激素的测定及其生态风险评估
胡红美(),李铁军(),张露,郝青,孙秀梅,金衍健,应忠真,郭远明
浙江省海洋水产研究所，浙江省海洋渔业资源可持续利用技术研究重点实验室，浙江 舟山 316021
Determination and ecological risk assessment of phthalic acid esters in marine sediments
Hongmei HU(),Tiejun LI(),Lu ZHANG,Qing HAO,Xiumei SUN,Yanjian JIN,Zhongzhen YING,Yuanming GUO
Key Laboratory of Sustainable Utilization of Technology Research for Fisheries Resources of Zhejiang Province, Marine Fishery Institute of Zhejiang Province, Zhoushan 316021, Zhejiang, China
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摘要：

本研究建立了一种对海洋沉积物中16种邻苯二甲酸酯（phthalic acid esters, PAEs）的超声波萃取-分散固相萃取净化-气相色谱质谱检测法，并采用该方法对台州三门湾海域、温州南麂岛海域采集的样品进行检测，同时对其生态风险进行了评估。结果表明：该方法线性范围为1～1 000 μg/L，相关系数为0.999 1～0.999 9，检出限（3倍信噪比）为0.10～0.25 μg/kg，不同浓度的加标回收率为75%～116%，相对标准偏差（n=5）为3.1%～7.2%。组分分析表明，PAEs总量为297.43～550.25 μg/kg，以邻苯二甲酸二异丁酯（diisobutyl phthalate, DIBP）、邻苯二甲酸二丁酯（di-n-butyl phthalate, DBP）、邻苯二甲酸二-2-乙基己酯[di (2-ethylhexyl) phthalate, DEHP]为主，占PAEs总量的88.7%～96.7%。基于质量基准法的生态风险评估表明，各采样点的沉积物中PAEs含量均小于相应的环境风险限值，生态风险总体较低。基于风险商值法的评价表明：PAEs对水生生物的风险大小顺序为DBP＞DIBP＞DEHP，其中DBP对藻类呈高风险，对甲壳类和鱼类为中等风险，DIBP对甲壳类为中等风险，DEHP对水生生物均为低风险；PAEs对藻类的风险最大，其次为甲壳类，对鱼类的风险最小。总体上，台州三门湾海域PAEs对水生生物的风险略高于温州南麂岛海域。

关键词： 超声波萃取;  分散固相萃取净化;  气相色谱质谱法;  沉积物;  邻苯二甲酸酯;  生态风险评估    
Abstract:

We proposed a new method for the determination of 16 phthalic acid esters (PAEs) in marine sediments using gas chromatography-mass spectrometry (GC-MS) combined with ultrasonic extraction and dispersive solid phase extraction cleanup. Moreover, the contents of PAEs in marine sediments of Sanmen Bay, Taizhou and waters of Nanji Island, Wenzhou were detected and their ecological risk was assessed. Under the optimized condition, the linearity of this method ranged from 1 to 1 000 μg/L, with regression coefficients ranging between 0.999 1 and 0.999 9. The limits of detection were in the rang of 0.10-0.25 μg/kg. The recoveries of spiked 16 PAEs at different concentration levels were in the range of 75%-116%, with relative standard deviations of 3.1%-7.2%. The results showed that the total concentration of phthalate esters ranged from 297.43 to 550.25 μg/kg. Diisobutyl phthalate (DIBP), di-n-butyl phthalate (DBP) and di (2-ethylhexyl) phthalate (DEHP) were the predominant compounds in all detected seafood, accounted for 88.7%-96.7% of the total PAEs. Marine sediment’s ecological risk was assessed with the methods of sediment quality guidline and risk quotient. The sediment quality guidline results showed the contents of PAEs in the sediments were all lower than the environmental risk limits, which indicated low ecological risk. The risk quotient values of PAEs were in the following order: DBP＞DIBP＞DEHP, and DBP was high risk to algae and medium risk to crustaceans and fish, and DIBP was medium risk to crustaceans, and DEHP was low risk to aquatic organisms. Overall, the risk of PAEs on algae was the largest, followed by crustaceans, minimal risk for fish, and the health risk of Sanmen Bay, Taizhou was slightly higher than that of waters of Nanji Island, Wenzhou.
Key words: ultrasonic extraction    dispersive solid phase extraction cleanup    gas chromatography-mass spectrometry    sediment    phthalic acid esters    ecological risk assessment
收稿日期: 2018-03-28 出版日期: 2019-06-25
CLC:  O 65  
基金资助: 国家自然科学基金(31800430);浙江省科技计划项目(2017F50021);浙江省科协育才项目(2017YCGC013);浙江省舟山市科技项目(2016C31055)
通讯作者: 李铁军     E-mail: huhm@zju.edu.cn;tiejun82_li@126.com
作者简介: 胡红美（https://orcid.org/0000-0003-3750-3755），E-mail：huhm@zju.edu.cn
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胡红美
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引用本文:

胡红美,李铁军,张露,郝青,孙秀梅,金衍健,应忠真,郭远明. 海洋沉积物中邻苯二甲酸酯类环境激素的测定及其生态风险评估[J]. 浙江大学学报（农业与生命科学版）, 2019, 45(3): 365-375.

Hongmei HU,Tiejun LI,Lu ZHANG,Qing HAO,Xiumei SUN,Yanjian JIN,Zhongzhen YING,Yuanming GUO. Determination and ecological risk assessment of phthalic acid esters in marine sediments. Journal of Zhejiang University (Agriculture and Life Sciences), 2019, 45(3): 365-375.

链接本文:

http://www.zjujournals.com/agr/CN/10.3785/j.issn.1008-9209.2018.03.282    或    http://www.zjujournals.com/agr/CN/Y2019/V45/I3/365

峰号

Peak No.

化合物

Compound

保留时间

Retention time/min

定量离子

Quantitative ion (m/z)

定性离子

Qualitative ions (m/z)
1 DMP 8.354 163 77，135，194
2 DEP 9.793 149 121，177，222
3 DIBP 12.380 149 167，205，223
4 DBP 13.452 149 121，205，223
5 BMPP 14.076 149 104，167，251
6 DMEP 14.467 59 104，149，207
7 DNPP 15.162 149 104，219，237
8 DEEP 15.315 72 104，149，193
9 DNHP 16.751 149 104，167，251
10 BBP 17.643 149 91，104，206
11 DEHP 18.073 149 104，167，279
12 DBEP 18.145 149 85，101，193
13 DCHP 18.991 149 55，167，249
14 DNOP 19.714 149 167，261，279
15 DPhP 19.893 225 77，153，197
16 DNP 21.566 149 55，167，293
表1  16种PAEs的保留时间、定量离子和定性离子
图1   16种PAEs混合标准溶液的总离子图
化合物Compound 种群Population 物种名Species name C PNE/(μg/g)
DNP 甲壳类Crustaceans Nitocra spinipes 0.732
DMP 藻类Algae Skeletonema costatum 0.134
甲壳类Crustaceans Americamysis bahia 0.098
鱼类Fish Cyprinodon variegatus 0.078
DEP 藻类Algae Skeletonema costatum 1.219
甲壳类Crustaceans Americamysis bahia 0.024
鱼类Fish Cyprinodon variegatus 0.093
DIBP 甲壳类Crustaceans Nitocra spinipes 0.178
DBP 藻类Algae Karenia brevis 0.022
甲壳类Crustaceans Nitocra spinipes 0.189
鱼类Fish Rivulus marmoratus 0.111
BBP 藻类Algae Skeletonema costatum 0.007
甲壳类Crustaceans Americamysis bahia 0.021
鱼类Fish Cyprinodon variegatus 0.012
DEHP 藻类Algae Karenia brevis 1 010 519.000
甲壳类Crustaceans Americamysis bahia 32.597
鱼类Fish Oryzias melastigma 32.597
表2  海洋沉积物中PAEs的预测无影响浓度
图2  不同萃取剂对PAEs的萃取效果比较
图3  不同吸附剂对PAEs的净化效果比较
图4  不同固相吸附剂净化时PAEs的总离子流色谱图

峰号

Peak No.

化合物

Compound

线性回归方程

Linear regression equation

相关系数

Correlation coefficient

检出限

Detection limit/(μg/kg)
1 DMP y＝95.58x－43.52 0.999 3 0.10
2 DEP y＝88.71x－62.64 0.999 2 0.10
3 DIBP y＝136.25x－101.28 0.999 4 0.10
4 DBP y＝162.48x－68.42 0.999 3 0.10
5 BMPP y＝35.71x－11.05 0.999 1 0.15
6 DMEP y＝32.45x－25.65 0.999 8 0.20
7 DNPP y＝159.37x＋17.80 0.999 3 0.10
8 DEEP y＝24.21x－18.21 0.999 5 0.20
9 DNHP y＝145.23x－118.51 0.999 2 0.10
10 BBP y＝59.62x－42.87 0.999 3 0.15
11 DEHP y＝77.01x－65.15 0.999 1 0.15
12 DBEP y＝24.21x－15.65 0.999 6 0.25
13 DCHP y＝93.28x－62.58 0.999 4 0.15
14 DNOP y＝94.15x－79.51 0.999 9 0.20
15 DPhP y＝107.12x－55.58 0.999 9 0.20
16 DNP y＝60.12x－47.88 0.999 4 0.20
表3  16种PAEs的线性回归方程、相关系数和检出限

峰号

Peak No.

化合物

Compound

 背景值Background

加标水平Spiked level

(5 μg/kg)

加标水平Spiked level

(50 μg/kg)

加标水平Spiked level

(250 μg/kg)

平均值

Mean/(μg/kg)

 RSD/%

回收率

Recovery/%

 RSD/%

回收率

Recovery/%

 RSD/%

回收率

Recovery/%

 RSD/%
1 DMP 10.42 3.2 101 3.6 75 3.4 81 3.2
2 DEP 1.32 4.3 104 4.5 85 3.3 92 3.5
3 DIBP 74.20 3.5 113 3.8 98 3.2 96 4.0
4 DBP 44.32 3.9 116 4.2 95 3.8 87 3.2
5 BMPP ND 112 3.8 105 3.6 101 3.9
6 DMEP ND 106 4.3 107 3.5 106 3.2
7 DNPP ND 112 4.2 106 3.1 98 3.2
8 DEEP ND 101 4.1 98 3.5 95 3.4
9 DNHP ND 111 3.2 113 4.4 103 3.2
10 BBP ND 107 3.5 110 3.9 98 3.1
11 DEHP 225.96 5.2 112 7.2 107 6.3 101 5.8
12 DBEP ND 105 4.4 103 4.7 99 3.7
13 DCHP ND 109 4.1 110 4.2 95 3.8
14 DNOP ND 110 3.6 86 3.5 92 3.5
15 DPhP ND 105 4.1 95 3.5 94 3.3
16 DNP ND 98 4.5 88 3.3 88 3.2
表4  精密度和回收试验结果

峰号

Peak No.

 化合物Compound 台州三门湾海域 Sanmen Bay, Taizhou 温州南麂岛海域Waters of Nanji Island, Wenzhou
样品1 Sample 1

样品2

Sample 2

样品3

Sample 3

样品1

Sample 1

样品2

Sample 2

样品3

Sample 3
方正汇总行∑16 PAEs 490.98 433.46 550.25 297.43 356.22 448.61
1 DMP 26.72 40.79 39.60 12.67 10.42 20.40
2 DEP 4.13 4.46 8.22 1.95 1.32 2.80
3 DIBP 98.79 95.72 200.92 69.03 74.20 93.12
4 DBP 78.21 53.88 78.46 35.13 44.32 63.14
5 BMPP ND ND ND ND ND ND
6 DMEP ND ND ND ND ND ND
7 DNPP ND ND ND ND ND ND
8 DEEP ND ND ND ND ND ND
9 DNHP ND ND ND ND ND ND
10 BBP ND ND ND ND ND ND
11 DEHP 277.98 235.01 216.12 177.97 225.96 265.84
12 DBEP ND ND ND ND ND ND
13 DCHP ND ND ND ND ND ND
14 DNOP ND ND ND ND ND ND
15 DPhP ND ND ND ND ND ND
16 DNP 5.15 3.60 6.93 0.68 ND 3.31
表5  样品分析结果
图5  不同采样点采集的海洋沉积物中PAEs组分特征

采样点

Sampling point

种群

Population

 风险商值（范围，平均值） Risk quotient (range, mean)
DMP DEP DIBP DBP DEHP

台州三门湾海域

Sanmen Bay, Taizhou

藻类

Algae

 0.20～0.30, 0.27 0.003～0.007, 0.005 ND 2.45～3.57, 3.19 2.1×10－7～2.8×10－7, 2.4×10－7

甲壳类

Crustaceans

 0.27～0.42, 0.36 0.17～0.34, 0.23 0.54～1.13, 0.74 0.29～0.42, 0.37 0.007～0.009, 0.007

鱼类

Fish

 0.34～0.52, 0.45 0.04～0.09, 0.06 ND 0.49～0.71, 0.63 0.007～0.009, 0.007

温州南麂岛海域

Waters of Nanji Island, Wenzhou

藻类

Algae

 0.08～0.15, 0.11 0.001～0.002, 0.002 ND 1.60～2.87, 2.16 1.8×10－7～2.6×10－7, 2.2×10－7

甲壳类

Crustaceans

 0.11～0.21, 0.15 0.06～0.12, 0.08 0.39～0.52, 0.44 0.19～0.33, 0.25 0.005～0.008, 0.007

鱼类

Fish

 0.13～0.26, 0.19 0.01～0.03, 0.02 ND 0.32～0.57, 0.43 0.005～0.008, 0.007
表6  海洋沉积物中5种PAEs的风险商值（Q R）
图6  不同采样点采集的海洋沉积物中5种PAEs对不同水生生物 ∑ Q R 的影响
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