北京清河水体中有机磷酸酯的污染特征与生态风险评估

雷啟焘; 史亚利; 汤智; 牛琳; 赵晓丽

doi:10.13198/j.issn.1001-6929.2023.01.13

北京清河水体中有机磷酸酯的污染特征与生态风险评估

doi: 10.13198/j.issn.1001-6929.2023.01.13

雷啟焘^{1, 2,},
史亚利²,
汤智¹,
牛琳¹,
赵晓丽^1, ,

1.
中国环境科学研究院，环境基准与风险评估国家重点实验室，北京　100012
2.
中国科学院生态环境研究中心，环境化学与生态毒理学国家重点实验室，北京　100083

基金项目: 国家自然科学基金项目(No.41991315)

详细信息

作者简介:
雷啟焘（1993-），男，浙江衢州人，leiqitao@126.com

通讯作者:
赵晓丽(1981-)，女，河北邢台人，研究员，博士，博导，主要从事水质基准理论与方法学和纳米材料研究，zhaoxiaoli_zxl@126.com

中图分类号: X83
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出版历程
- 收稿日期: 2022-11-10
- 修回日期: 2023-01-28

Pollution Characteristics and Ecological Risk Assessment of Organophosphate Esters in Qinghe River, Beijing

LEI Qitao^{1, 2
,},
SHI Yali²,
TANG Zhi¹,
NIU Lin¹,
ZHAO Xiaoli^{1
, ,}

1.
State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing 100012, China
2.
State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environment, Chinese Academy of Sciences, Beijing 100083, China

Funds: National Natural Science Foundation of China (No.41991315)

摘要

摘要: 为了探究城市地表水中有机磷酸酯(OPEs)污染水平和生态风险，采用超高效液相色谱-质谱联用仪(UPLC-MS/MS)分析测定了北京清河地表水中10种OPEs的浓度水平和成分组成，使用相关性分析和主成分分析对地表水中OPEs进行源解析，并评估生态风险. 结果表明：北京清河地表水中∑₁₀OPEs浓度范围为439.61~1 053.06 ng/L，浓度中位值为768.85 ng/L，平均值为761.77 ng/L，其中磷酸三(1-氯-2-丙基)酯(TCIPP)以及磷酸三(1-氯-2-丙基)酯(TCEP)是主要污染物. ∑₁₀OPEs浓度沿河流方向呈先稳定后降低再缓慢升高的特征. 源解析结果表明，污水处理厂、道路交通、建筑装饰材料及汽车维修可能是北京清河地表水中OPEs的主要来源. 风险熵评估结果表明，水体中TCEP等10种OPEs的生态风险相对较低，但其引起的联合效应值得进一步关注. 研究显示，北京清河地表水中OPEs污染水平相对较高，受人为活动影响较大，造成的生态风险可以忽略.
- 有机磷酸酯(OPEs) /
- 源解析 /
- 生态风险
Abstract: In order to explore the pollution characteristics, potential sources and ecological risk of organophosphate esters (OPEs) in urban surface water, the concentrations of 10 species of OPEs in the surface water were determined using UPLC-MS/MS. The potential sources, ecological risk and spatial distribution of the OPEs in surface water of the Qinghe River was further analyzed. The pollution sources were analyzed by correlation analysis and principal component analysis, and the ecological risk was evaluated. The results showed that the concentration of ∑₁₀OPEs in surface water ranged from 439.61 to 1053.06 ng/L, the median concentration of 768.85 ng/L and the average concentration of 761.77 ng/L. Tri(1-chloro-2-propyl) phosphate (TCIPP) and tri(1-chloro-2-propyl) phosphate (TCEP) were the main pollutants. The distribution of ∑₁₀OPEs showed an obvious regional pattern, which was steady first, then decreased and then increased slowly along the direction of the Qinghe River inlet. The source analysis results revealed that sewage treatment plant, road traffic, building decoration materials and vehicle maintenance were the sources of OPEs in the surface water of the Qinghe River. The ecological risk assessment results indicate that the risk of 10 OPEs to aquatic organisms in the Qinghe River was low, but their combined effects deserved further attention. The research shows that the surface water of the Qinghe River is highly polluted by OPEs, it is greatly affected by human activities, and the ecological risks caused can be ignored.
- organophosphate esters (OPEs) /
- source analysis /
- ecological risk

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图 1 北京清河水样采集点示意

Figure 1. Sampling sites of surface water in Qinghe River, Beijing

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图 2 北京清河各采样点OPES的浓度与组成

Figure 2. Concentration and composition of OPEs at each sampling site in Qinghe River, Beijing

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图 3 Spearman相关性分析

注：*表示在P<0.05水平上(双尾)显著相关.

Figure 3. Spearman correlation analysis

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图 4 主成分分析因子载荷与得分

Figure 4. Loading and score plot of the PCA

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图 5 北京清河各采样点OPEs风险熵值

Figure 5. RQ of the OPEs in the sampling sites in in Qinghe River, Beijing

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表 1 OPEs的分子式、相对分子质量及CAS号

Table 1. Formulas, relative molecular masses and CAS numbers of OPEs

化合物	英文缩写	化学式	相对分子质量	CAS号
Trimethyl phosphate(磷酸三甲酯)	TMP	C₃H₉O₄P	140.8	512-56-1
Triethyl phosphate(磷酸三乙酯)	TEP	C₆H₁₅O₄P	182.16	78-40-0
Tri-iso-butyl phosphate(磷酸三正丁酯)	TnBP	C₁₂H₂₇O₄P	266.31	126-73-8
Tri(2-butoxyethyl)phosphate(磷酸三丁氧酯)	TBEP	C₁₈H₃₉O₇P	398.47	78-51-3
Tri(2-chloroethyl)phosphate(磷酸三(2-氯乙基)酯)	TCEP	C₆H₁₂C_l3O₄P	285.49	115-96-8
Tri(1-chloro-2-propyl)phosphate(磷酸三(1-氯-2-丙基)酯)	TCIPP	C₉H₁₈C_l3O₄P	327.57	13674-84-5
Tri(1,3-dichloro-2-propyl)phosphate(磷酸三(1,3-二氯-2-丙基)酯)	TDCP	C₉H₁₅C_l6O₄P	430.90	13674-87-8
Trimethylphenyl phosphate(磷酸三甲苯酯)	TCrP	C₂₁H₂₁O₄P	368.36	563-04-2
Cresyl diphenyl phosphate(磷酸甲苯二苯酯)	CDPP	C₁₉H₁₇O₄P	340.31	26444-49-5
2-Ethylhexyl di-phenyl phosphate(2-乙基己基苯基磷酸酯)	EHDPP	C₂₀H₂₇O₄P	340.31	1241-94-7

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表 2 目标化合物离子对及相应质谱参数

Table 2. Analyte ions and MS parameters of target OPEs

化合物	保留时间/min	母离子 (m/z)	子离子 (m/z)	去簇电压/V	碰撞能/V
TMP	1.66	140	78	30	22
TMP	1.66	140	108	30	18
TEP	2.01	182	98¹⁾	25	18
TEP	2.01	182	126	25	12
TCEP	2.39	286	98¹⁾	42	24
TCEP	2.39	286	124	42	14
TnBP	3.9	266	98	26	15
TnBP	3.9	266	155	26	8
TCIPP	2.98	328	247¹⁾	2	8
TCIPP	2.98	328	288	2	2
CDPP	4.37	341	152	39	39
EHDPP	6.82	363	251	31	39
EHDPP	6.82	363	91	30	6
TBEP	4.58	399	199	2	14
TBEP	4.58	399	299	2	12
TCrP	5.77	368	91	98	32
TCrP	5.77	368	165	98	32
TDCP	3.68	429	99	24	26
TDCP	3.68	429	98	32	20
TPrP-_d21	2.74	246	101¹⁾	36	18
TPrP-_d21	2.74	246	150	36	10
TnBP-_d27	3.86	294	101¹⁾	36	18
TnBP-_d27	3.86	294	166	36	12
TCIPP-_d18	2.95	346	101¹⁾	36	20
TCIPP-_d18	2.95	346	183	36	10
注：1)表示定量离子.

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表 3 OPEs的加标回收率、相关系数、检出限和定量限

Table 3. Spiked recoveries, correlation coefficient, limits of detection and limits of quantitation of OPEs

化合物	加标回收率±标准差(n=3)	相关系数(R²)	检出限/ (ng/L)	定量限/ (ng/L)
TMP	90.2%±4.3%	0.998	0.33	1.10
TEP	87.3%±9.9%	0.999	0.35	1.17
TCEP	95.2%±3.7%	0.995	0.78	2.60
TnBP	83.6%±5.2%	0.995	0.33	1.10
TCIPP	101.2%±8.4%	0.994	0.57	1.90
CDPP	89.5%±6.1%	0.998	0.21	0.70
EHDPP	81.4%±5.4%	0.996	0.44	1.47
TBEP	90.2%±7.1%	0.994	0.12	0.40
TCrP	95.3%±7.4%	0.995	0.55	1.83
TDCP	96.5%±4.4%	0.998	0.13	0.43

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表 4 北京清河OPEs的总体检出水平

Table 4. Summary of OPEs concentration in the sampled surface water in Qinghe River, Beijing

目标物质	检出率/%	浓度/(ng/L)				含量/%
目标物质	检出率/%	最大值	最小值	平均值	中位值	含量/%
TMP	100	37.98	13.01	21.85	20.08	2.87
TEP	100	77.64	39.84	58.38	57.97	7.66
TnBP	100	34.02	14.09	26.21	26.02	3.44
TBEP	100	27.90	3.74	7.02	5.32	0.92
TCEP	100	190.44	86.77	135.06	136.07	17.73
TCIPP	100	598.97	260.13	457.76	468.43	60.09
TDCP	100	84.13	21.55	54.38	53.83	7.14
CDPP	100	0.78	0.10	0.45	0.49	0.06
EHDPP	100	0.69	0.18	0.32	0.30	0.04
TCrP	100	0.51	0.21	0.33	0.33	0.04
∑₁₀OPEs	—	1 053.06	439.61	761.77	768.85	—

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表 5 国内外河流、湖泊和海水中OPEs浓度对比

Table 5. Concentration of OPEs in different rivers, lakes and seawater around the world

国家	河流/湖泊	ΣOPEs浓度/(ng/L)	烷基类OPEs浓度/(ng/L)				氯代OPEs浓度/(ng/L)			烷基类OPEs浓度/(ng/L)			数据来源
国家	河流/湖泊	ΣOPEs浓度/(ng/L)	TMP	TEP	TnBP	TBEP	TCEP	TCIPP	TDCP	TCrP	EHDPP	CDPP	数据来源
中国	北京清河	761.77 (439.61~1053.06)	21.85 (13.01~37.98)	58.38 (39.84~77.64)	26.21 (14.09~34.02)	7.02 (3.74~27.90)	135.06 (86.77~190.44)	457.76 (260.13~598.97)	54.38 (21.55~84.13)	0.33 (0.21~0.51)	0.32 (0.18~0.69)	0.45 (0.10~0.78)	该研究
中国	珠江三角洲河流	160(25~840)	—	11.0 (4.17~33.4)	11 (<LOD~360)	12 (<LOD~32)	17 (<LOD~150)	120 (22~330)	10 (<LOD~99)	—	24 (<LOD~480)	—	文献[32]
中国	北京城区河流	954 (3.24~10 945)	144 (<LOD~9497)	88.7 (nd~2072)	19.6 (nd~256)	<LOD~3617	219 (nd~5689)	291 (nd~1742)	46.3 (nd~855)	0.18 (<LOD~4.29)	0.38 (<LOD~40.3)	0.43 (<LOD~4.85)	文献[1]
中国	太湖	800 (100~1700)	28 (2.7~84)	620 (53~1400)	—	0.11 (nd~2.7)	44 (14~76)	93 (12~290)	1.8 (nd~6.0)	0.088 (nd~1.5)	2.8 (0.88~12)	—	文献[8]
中国	骆马湖	127 (0.82~708)	25.2 (<LOD~127)	11.7 (nd~32.1)	2.37 (0.01~5.85)	0.07 (0.002~0.18)	69.6 (0.01~552)	5.79 (0.02~10.8)	0.95 (0.03~1.98)	6.36 (0.71~54.6)	1.86 (<LOD~3.39)	—	文献[33]
中国	上海城区河流	850 (339~1689)	—	—	29.9 (11.6~63.3)	46.6 (15.9~100.6)	348.5 (67.5~865.2)	259 (123.9~523)	25.1 (<LOD~45.3)	—	—	—	文献[6]
中国	上海郊区河流	222 (185~321)	—	—	25 (6.9~44.8)	23.6 (<LOD~47.9)	38.2 (30~63.3)	77.4 (60~154.2)	<LOD	—	—	—	文献[6]
中国	成都锦江	3747.58 (689.09~10 623.94)	—	—	36.16~85.41	274.25~ 10 186.61	27.68~273.10	35.76~143.75	—	—	—	—	文献[27]
中国	环渤海40条河流	300 (9.6~1549)	—	—	<LOD~81	<LOD~47	1~268	5~921	<LOD~44	—	—	—	文献[7]
中国	广州蕉门水道	442±6.66	—	33.4±0.85	64.9±1.83	—	102±3.62	215±7.43	5.43±0.17	nd	—	—	文献[26]
中国	中山横门水道	217±3.84	—	5.17±0.11	125±2.61	—	28.8±0.78	32.3±1.23	2.72±0.11	nd	—	—	文献[26]
中国	广州红旗门水道	178±4.17	—	7.44±0.32	60.4±2.52	—	47.6±3.39	42.1±0.75	2.53±0.06	nd	—	—	文献[26]
中国	广州虎门水道	193±1.98	—	4.17±0.14	49.0±2.40	—	35.7±0.69	77.8±3.17	4.67±0.10	nd	—	—	文献[26]

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续表 5
国家	河流/湖泊	ΣOPEs浓度/ (ng/L)	烷基类OPEs浓度/(ng/L)				氯代OPEs浓度/(ng/L)			烷基类OPEs浓度/(ng/L)			数据来源
国家	河流/湖泊	ΣOPEs浓度/ (ng/L)	TMP	TEP	TnBP	TBEP	TCEP	TCIPP	TDCP	TCrP	EHDPP	CDPP	数据来源
中国	湘江水源地	14.9 (6.07~25.3)	—	—	—	—	0.23 (nd~0.46)	6.83 (2.04~13.5)	—	—	0.61 (0.45~0.99)	—	文献[34]
中国	洞庭湖旱季湖水	49.5~148	—	—	1.87 (1.04~2.56)	<LOD	7.89 (2.26~12.6)	6.00 (1.64~6.05)	0.590 (<LOD~0.871)	—	—	—	文献[35]
中国	洞庭湖雨季湖水	5.00~45.7	—	—	12.5 (<LOD~23.5)	<LOD	31.6 (16.7~44.5)	43.8 (27.3~106)	3.46 (<LOD~6.59)	—	—	—	文献[35]
中国	莱州湾海水	88.4±5.3	6.0±2.4	3.9±1.2	15.2±5.0	11.7±5.7	5.5±1.5	18.8±5.1	1.6±1.0	0.6±0.4			文献[36]
加拿大	北冰洋	11 (0.017~306)	—	—	0.55 (<LOD~8.1)	<LOD	5.5 (<LOD~246)	2.9 (0.17~53)	—	—	0.13 (<LOD~7.0)	—	文献[37]
美国	Michigan湖	8.6~10	—	—	0.45~0.77	—	0.30~0.46	2.9~3.2	0.92~1.3	—	—	—	文献[38]
英国	Aire 河	—	—	—	—	—	119~316	6 040 (113~26 050)	62~149	—	—	—	文献[9]
欧洲	Danube 河	1 014.6	—	—	5.6 (0.4~700)	13 (<LOQ~93)	119 (2.4~4.1)	115 (28~603)	11 (nd~28)	—	0.6 (<LOQ~5.9)	—	文献[39]
韩国	Shihwa 河	2344 (597~16 000)	—	459 (42.2~3 677)	40.3 (15.6~72.9)	436 (145~839)	706 (86.5~5 963)	594 (68.3~5 102)	48.1 (<LOD~325)	—	9.87 (1.91~59.2)	—	文献[25]
美国	Hudson 河	191 (37.2~510)	0.49 (<LOQ~3.97)	4.77 (<LOQ~24.8)	—	66.2 (2.53~366)	14.6 (<LOQ~79.5)	74.6 (3.30~214)	21.1 (<LOQ~86.7)	—	—	—	文献[40]
西班牙	Nalón 河、Arga 河、 Besòs 河	7.6~7 200	—	—	<LOD~370	<LOD~4 600	<LOD~330	<LOD~1 800	<LOD~200	<LOD~0.009 2	<LOD~0.046	—	文献[41]
奥地利	Danube 河、Schwechat 河、Liesig 河	141~922	—	13~51	—	24~500	13~130	33~170	<MLQ~19	nd	—	—	文献[42]
注：括号中数值为OPEs总浓度范围. <LOD表示小于检出限，<LOQ表示小于定量限，nd表示未检出，—表示无数据.

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表 6 OPEs毒理数据及生态风险

Table 6. Toxicity data and ecological risk of OPEs

化合物	敏感物种	LC₅₀/(mg/L)	PNEC/(mg/L)	RQ_S
TMP	藻类(Scenedesmus subspicatus)	—	—	—
	甲壳类(Daphnia magna)	—	—	—
	鱼类(Pimephales promelas)	7 000	7 000 000	0.000 002~0.000 005
TEP	藻类(Scenedesmus subspicatus)	900	900 000	0.000 044~0.000 086
	甲壳类(Daphnia magna)	350	350 000	0.000 114~0.000 222
	鱼类(Leuciscus idus)	2 140	2 140 000	0.000 019~0.000 036
TnBP	藻类(Scenedesmus subspicatus)	34	34 000	0.000 414~0.001 001
	甲壳类(Daphnia magna)	11	11 000	0.001 280~0.003 093
	鱼类(Leuciscus idus)	20	20 000	0.000 704~0.001 701
TBEP	藻类(Scenedesmus subspicatus)	—	—	—
	甲壳类(Daphnia magna)	75	75 000	0.000 050~0.000 372
	鱼类(Pimephales promelas)	13	13 000	0.000 288~0.002 146
TCEP	藻类(Scenedesmus subspicatus)	51	51 000	0.001 807~0.003 734
	甲壳类((Daphnia magna)	330	330 000	0.000 263~0.000 577
	鱼类(Carassius auratus)	90	90 000	0.000 964~0.002 116
TCIPP	藻类(Scenedesmus subspicatus)	45	45 000	0.005 780~0.013 310
	甲壳类(Daphnia magna)	91	91 000	0.002 859~0.006 582
	鱼类(Poecilia reticulata)	30	30 000	0.008 671~0.019 966
TDCP	藻类(Pseudokirchneriella subcapitata)	39	39 000	0.000 553~0.002 157
	甲壳类(Daphnia magna)	4.2	4 200	0.005 130~0.020 032
	鱼类(Carassius auratus)	5.1	5 100	0.004 225~0.016 497
CDPP	藻类(Scenedesmus subspicatus)	0.6	600	0.000 167~0.001 301
	甲壳类(Daphnia magna)	—	—	—
	鱼类(Pimephales promelas)	—	—	—
EHDPP	藻类(Scenedesmus subspicatus)	—	—	—
	甲壳类(Daphnia magna)	0.018	18	0.009 880~0.038 277
	鱼类(Pimephales promelas)	—	—	—
TCrP	藻类(Scenedesmus subspicatus)	0.29	290	0.000 731~0.001 737
	甲壳类(Daphnia magna)	0.27	270	0.000 786~0.001 884
	鱼类(Lepomis macrochirus)	0.11	110	0.001 928~0.004 623
注：“—”表示未查询或计算到相关数据.

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参考文献(48)

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