CN106841431A - PPCPs ecological risk evaluating methods in a kind of water environment - Google Patents

PPCPs ecological risk evaluating methods in a kind of water environment Download PDF

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CN106841431A
CN106841431A CN201710024798.7A CN201710024798A CN106841431A CN 106841431 A CN106841431 A CN 106841431A CN 201710024798 A CN201710024798 A CN 201710024798A CN 106841431 A CN106841431 A CN 106841431A
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concentration
ppcps
water
risk
environment
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赵新华
王晓欧
吴卿
张练
肖敏如
李楠
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Tianjin University
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
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    • G01N2030/027—Liquid chromatography

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Abstract

The invention discloses PPCPs ecological risk evaluating methods in a kind of water environment：(1) PPCPs concentration in detection water environment, including three steps：Water sample pretreatment, SPE and carry out quantitative determination using high performance liquid chromatography mass spectrometric hyphenated technique；(2) with aquatic organisms such as bacterium, algae, invertebrate and fish as biological subject, using half effective concentration (50%effective concentration, EC50) this toxicology data determine prediction without effective concentration (Predicted No Effect Concentration, PNEC) value；(3) by formula RQ=MEC/PNEC calculation risks quotient (Risk Quotients, RQ), wherein MEC is the concentration (Measured Environmental Concentration) detected in environment；(4) the ecological risk degree of target PPCPs compounds is assessed using risk quotient method.Low cost of the present invention, it is environment-friendly, be easy to operation, wherein operation is simple for the detection method of PPCPs, and, sensitivity strong to the selectivity of target compound is high, and enrichment times are high, favorable reproducibility, being capable of separation determination multiple compounds simultaneously.

Description

PPCPs ecological risk evaluating methods in a kind of water environment
Technical field
In particular it is PPCPs lifes in a kind of water environment the present invention relates to environmental science and ecological risk assessment field State risk evaluating method.
Background technology
At present, medicine and personal care articles (Pharmaceuticals and Personal Care Products, PPCPs water environment pollution problem) has caused international community's extensive concern.PPCPs is that a class is contacted most with people's daily life It is close emerging pollutant, comprising various chemical substances, mainly including medicine (human administration such as antibiotic, anti-inflammatory With medicine, calm medicine, anti-epileptic medicine, analgesic thing, step-down medicine, contraception medicine, hypnosis medicine etc. And veterinary drug), personal care articles (the chemical consumer goods, such as cosmetics, suncream, hair dye, Moschus class material, cleaning disinfectant Deng) and the various additives that use and inert fraction etc. in medicine and nursing product production and process.
PPCPs products various fields to widely use the approach that causes it to enter environment varied.First in production Link, during PPCPs can be directly discharged to environment in the form of producing waste water, waste, directly pollution is caused to environment；Secondly exist When using, PPCPs products are not fully absorbed by mankind's use or after taking in, considerable part is directly with the shape of parent compound Formula is drained with urine, excrement etc., and these compounds enter sewage treatment plant with municipal wastewater, and traditional sewage disposal work Skill is limited to the removal efficiency of PPCPs pollutants, thus PPCPs is eventually discharged with sewage effluents, so as to earth's surface The water body environments such as water, underground water are polluted.Sewage treatment plant is the topmost source of PPCPs pollutants in water body environment. Additionally, the improper treatment of aquatic products livestock-raising, rainfall runoff and expired or discarded PPCPs class articles is dirty PPCPs classes The possible approaches that dye thing enters in environment.Although the half-life short of PPCPs, concentration it is low (concentration generally ng/L to μ g/L it Between), but because the injection of PPCPs continuation causes " false persistent pollution ", ecological environment and human health can all be caused to dive Threat.In recent years, domestic and international researcher detected to the PPCPs in different type water body, municipal sewage, earth's surface The presence of PPCPs pollutants is all detected in water, underground water even drinking water.Therefore, to the life of PPCPs pollutants in water environment State risk is correctly assessed, for predicting the pollution level of PPCPs and formulating prevention and control measures that PPCPs pollutes, tool There is very important realistic meaning.
Ecological risk characterizing method general in the world at present has quotient method, probabilistic risk assessment method and multi-level risk Evaluation assessment.All in all, the ecological risk assessment for PPCPs pollutants in water environment not yet forms perfect risk assessment System, the especially selection of PPCPs pollutant kinds are very little.
The content of the invention
The purpose of the present invention, is directed to the situation of the not perfect enough formation of PPCPs ecological risk assessments in current water environment, carries For PPCPs ecological risk evaluating methods in a kind of water environment, can quantitative analysis PPCPs pollutants ecological risk level, be The risk management of PPCPs classes material provides scientific basis in water environment.
The present invention is achieved by following technical solution.
PPCPs ecological risk evaluating methods in a kind of water environment, with following steps：
(1) PPCPs concentration in detection water environment
(1.1) water sample pretreatment：After collection water sample, the dosage according to 2.5g ascorbic acid/L water samples is anti-to being added in water sample Bad hematic acid, is quenched the chlorine residue in water sample；Water sample, the suspension in removal water sample are filtered using the polyethersulfone membranes that aperture is 0.2 μm Thing；According still further to 0.5g Na2The dosage of EDTA/L water samples in water sample to adding Na2EDTA, the metal ion in complexing water sample；Finally It is 2 to adjust water sample pH using hydrochloric acid；
(1.2) SPE：Methyl alcohol, ultrapure water water-supply-pipe are used successively, load onto HLB solid phase extraction columns, then successively Using 6mL Chromatographic Pure Methanols, 6mL 0.25g/L Na2The EDTA aqueous solution, 6mL ultra-pure waters are activated to solid phase extraction column； Water sample in step (1.1) is crossed into post with the flow velocity of 5mL/min, water sample adds ultra-pure water to drench pillar after passing through completely Wash, solid phase extraction column is sucked and dried using vavuum pump, then it is right under gravity condition as eluant, eluent with 10mL methyl alcohol HLB solid phase extraction columns are eluted, and collect eluent, and eluant, eluent nitrogen therein is blown under water bath condition it is near dry, plus Enter 25 μ L 2mg/L's13C3Atrazine-the Atrazine of mark as internal standard, then with acetonitrile and the first of 0.1% mass concentration Aqueous acid by volume 1:9 mixing, resulting solution is redissolved to residue, and it is to be measured to be settled to 1mL；
(1.3) quantitative determination：The use of HPLC-MS method to medicine is that PPCPs carries out quantitative determination；
(1.4) standard curve is drawn, is determined with inner mark method ration
(1.5) concentration and recovery of standard addition of target PPCPs pollutants in water sample to be measured are calculated
(2) determine that prediction is Predicted No Effect Concentration without effective concentration, be abbreviated as PNEC values
With aquatic organisms as biological subject, PNEC values are calculated by long-term acute toxicology data；Use Toxicology data is lethal concentration for LC, is abbreviated as LC, inhibition concentration i.e. effective Concentration, is abbreviated as the apparent inhibition concentrations of EC or non-i.e. non-observed effect concentration, contracting It is written as NOEC；
(3) calculation risk quotient is Risk Quotients, is abbreviated as RQ
Risk quotient is the concentration i.e. Measured Environmental Concentration detected in environment, contracting MEC is written as with prediction without the effective concentration i.e. ratio of PNEC, computing formula is RQ=MEC/PNEC；
(4) ecological risk grade is assessed
The ecological risk degree of target PPCPs compounds is estimated using risk quotient method；RQ<This is represented when 0.01 Compound devoid of risk, 0.01≤RQ<0.1 represents that the compound has low-risk, 0.1≤RQ to environment<1 represents the compound pair There is medium risk in environment, RQ >=1 represents that the compound has excessive risk to environment.
The HPLC-MS method that the step (1) (1.3) uses, is using Agilent1200 liquid phases The triple level Four bar mass spectrographs of chromatogram-Agilent6410B determine the concentration of PPCPs, and wherein chromatographic column is Agilent ZORBAX Eclipse Plus C-18 chromatographic columns -2.1mm × 100mm, 1.8 μm；The triple mass spectrometric matter of level Four bar of Agilent6410B Spectral condition is as follows：
Ionization mode：ESI+, ion source temperature：100 DEG C, capillary voltage：4000V, EFI day with fog pressure：35.0psi.
The toxicology data that the step (2) uses is the half effective concentration 50%effective of inhibition concentration Concentration, EC50。
The biological subject of the step (2) is bacterium, algae, invertebrate or fish.
The present invention compared with prior art, has the following advantages that：
1. this method low cost, it is environment-friendly, be easy to operation.
2. in this method the detection method of PPCPs operation is simple, sensitivity strong to the selectivity of target compound Height, enrichment times are high, favorable reproducibility, can be while separation determination multiple compounds.
Specific embodiment
With reference to specific embodiment, the present invention will be further described, but protection scope of the present invention is not limited to following tools Body embodiment.
Specific embodiment with the raw water of certain city of northern China waterworks as object, with the Diclofenac in raw water, Bu Luo 6 kinds of compounds such as sweet smell, Ketoprofen, Bezafibrate, fenofibrate, Paxil are target PPCPs compounds, implement this hair It is bright.
Using PPCPs ecological risk evaluating methods in water environment of the invention, step is as follows：
(1) PPCPs concentration in detection water environment
(1.1) water sample pretreatment：Collection 1L water samples, to 2.5g ascorbic acid is added in water sample, are quenched the chlorine residue in water sample； Water sample, removal are filtered using the polyethersulfone membranes (Solution of the U.S. (Pall Corporation) production) that aperture is 0.2 μm Suspension in water sample；To addition 0.5g Na in water sample2EDTA, the metal ion in complexing water sample；Finally adjusted using hydrochloric acid Water sample pH is 2；
(1.2) SPE：Methyl alcohol, ultrapure water water-supply-pipe are used successively, load onto HLB solid phase extraction columns (Waters Company produces), then 6mL Chromatographic Pure Methanols, 6mL 0.25g/L Na are utilized successively2The EDTA aqueous solution, 6mL ultra-pure waters extract to solid phase Pillar is taken to be activated；Water sample in step (1.1) is crossed into post with the flow velocity of 5mL/min, water sample adds 6mL to surpass after passing through completely Pure water carries out drip washing to pillar, to solid phase extraction column be sucked and dried 30min using vavuum pump, then with 10mL methyl alcohol conducts Eluant, eluent is eluted under gravity condition to HLB solid phase extraction columns, and eluent is collected in 10mL glass round bottom pipes, and The eluant, eluent nitrogen in eluent is blown under 40 DEG C of water bath conditions near dry, adds 25 μ L 2mg/L's13C3The Atrazine of mark- Atrazine adds initial ratio mobile phase (10% acetonitrile/formic acid water (containing 0.1% formic acid) solution) to residual as internal standard Thing is stayed to be redissolved, and it is to be measured to be settled to 1mL；
(1.3) quantitative determination：Surveyed using the triple level Four bar mass spectrographs of Agilent1200 liquid chromatograies-Agilent6410B Determine the concentration of PPCPs；Chromatographic column：Agilent ZORBAX Eclipse Plus C-18 chromatographic columns -2.1mm × 100mm, 1.8 μm；The triple mass spectrometric Mass Spectrometry Conditions of level Four bar of Agilent6410B are as follows：
Ionization mode：ESI+, ion source temperature：100 DEG C, capillary voltage：4000V, EFI day with fog pressure：35.0psi； Detection pattern：Multiple-reaction monitoring (MRM).
Table 1 is the mass spectral analysis parameter of target PPCPs compounds in raw water of waterworks.
Table 1
(1.4) standard curve is drawn, is determined with inner mark method ration
The preparation of standard liquid：Various PPCPs standard items are weighed with assay balance, is dissolved with methyl alcohol, be configured to dense Spend single mark storing solution (PPCPs of methyl alcohol can not be dissolved in, dissolved with acetone) for 1000mg/L.Take a certain amount of coffee Cause and Atrazine, single mark storing solution of concentration respectively 1.5mg/L and 2mg/L is configured to methyl alcohol as solvent, stand-by.Take each The mono- mark μ L of storing solution 20 of PPCPs, methanol dilution is used after being well mixed, and is settled to 10mL, is prepared into the mixed mark storing solution of 2mg/L. Acetonitrile and formic acid water (containing 0.1% formic acid) are used with volume ratio 1:9 mixing are diluted as solvent to mixed mark storing solution, It is final be made into concentration be followed successively by 0.1,1,15,50,200, the standard liquid of 500ppb, be measured according to above-mentioned condition.With dense The ratio between degree is abscissa, and the ratio between each substance responds value and internal standard response are returned for ordinate, obtain standard curve, are used for The content of the target PPCPs pollutants in determination sample.
(1.5) concentration and recovery of standard addition of target PPCPs pollutants in water sample to be measured are calculated
Collection water sample, carries out pre-treatment and SPE, according to step (1.3) using step (1.1) and (1.2) to water sample High Performance Liquid Chromatography/Mass Spectrometry detection is carried out, using the standard curve in step (1.4), target in water sample to be measured is calculated The concentration of PPCPs pollutants.The rate of recovery：
R --- the rate of recovery, %；
C2 --- the concentration of PPCPs in mark-on water sample, μ g/L；
C1 --- the concentration of PPCPs in blank water sample, μ g/L；
CS --- add the concentration of standard liquid, μ g/L；
V2 --- add standard liquid volume of water sample, L；
V1 --- blank volume of water sample, L；
VS --- standard liquid volume, L.
Table 2 for target PPCPs compounds standard curve, linearly dependent coefficient, detection limit, quantitative limit, determine concentration and Rate of recovery scope.
Table 2
(2) determine prediction without effective concentration (Predicted No Effect Concentration, PNEC) value
With some aquatic organisms as biological subject, such as bacterium, algae, invertebrate and fish are imitated using half Answer concentration (50%effective concentration, EC50) this toxicology data is calculated PNEC values.
Table 3 is the EC of target PPCPs compounds in raw water of waterworks50Data and PNEC tables of data.
Table 3
Compound Biological subject Test-types PNEC(ng/L)
Diclofenac V.fischeri (bacterium) 9.70 9700
Brufen H.attenuata (invertebrate) 1.65 1650
Ketoprofen V.fischeri (bacterium) 15.6 15600
Bezafibrate Hydra attenuata (metazoa) 25.85 25850
Fenofibrate B.calyciflorus (invertebrate) 1.44 1440
Paxil D.magna (planktonic organism) 2.5 2500
(3) calculation risk quotient (Risk Quotients, RQ)
Risk quotient be environment in detect concentration (Measured Environmental Concentration, MEC) with ratio of the prediction without effective concentration (PNEC), computing formula is RQ=MEC/PNEC.
(4) ecological risk grade is assessed
The ecological risk degree of target PPCPs compounds is estimated using risk quotient method.RQ<This is represented when 0.01 Compound devoid of risk, 0.01≤RQ<0.1 represents that the compound has low-risk, 0.1≤RQ to environment<1 represents the compound pair There is medium risk in environment, RQ >=1 represents that the compound has excessive risk to environment.
Table 4 is the ecological risk grade assessment result of target PPCPs compounds in raw water of waterworks.
Table 4
Compound Diclofenac Brufen Ketoprofen Bezafibrate Fenofibrate Paxil
Risk quotient (RQ) 0.0196 0.3840 0.0116 0.0008 0.0341 0.0099
Risk class It is low It is medium It is low Nothing It is low Nothing
Analysis data above, in six kinds of compounds, the PNEC values of Bezafibrate are maximum, and numerical value is 25850ng/L, FENOBRATE Special PNEC values minimum, numerical value is 1440ng/L, i.e., under equivalent environment concentration, Bezafibrate is non-to the least risk of environment Greatest risk of the nobert to environment.From result of calculation as can be seen that because PPCPs concentration is relatively in the raw water of waterworks Height, therefore there is different degrees of risk to environment in six kinds of PPCPs compounds.In six kinds of compounds, the risk factor of brufen 0.384 is reached, i.e., the medium risk to environment structure need to take certain measure to control it, Diclofenac, ketone group cloth Lip river There is low-risk to environment in fragrant and fenofibrate, risk factor value is respectively 0.0196,0.0116 and 0.0341, two kinds of residue Compound, Bezafibrate and Paxil are to environment devoid of risk.Ecological risk evaluating method in the present invention is for assessment water ring The ecological risk degree of PPCPs is effective in border.

Claims (4)

1. PPCPs ecological risk evaluating methods in a kind of water environment, with following steps：
(1) PPCPs concentration in detection water environment
(1.1) water sample pretreatment：After collection water sample, dosage according to 2.5g ascorbic acid/L water samples in water sample to adding Vitamin C Acid, is quenched the chlorine residue in water sample；Water sample, the suspension in removal water sample are filtered using the polyethersulfone membranes that aperture is 0.2 μm；Again According to 0.5g Na2The dosage of EDTA/L water samples in water sample to adding Na2EDTA, the metal ion in complexing water sample；Finally use Hydrochloric acid regulation water sample pH is 2；
(1.2) SPE：Methyl alcohol, ultrapure water water-supply-pipe are used successively, load onto HLB solid phase extraction columns, then utilize successively 6mL Chromatographic Pure Methanols, 6mL 0.25g/L Na2The EDTA aqueous solution, 6mL ultra-pure waters are activated to solid phase extraction column；Will step Suddenly the water sample in (1.1) crosses post with the flow velocity of 5mL/min, and addition ultra-pure water carries out drip washing to pillar after water sample passes through completely, makes Solid phase extraction column is sucked and dried with vavuum pump, then it is solid to HLB under gravity condition as eluant, eluent with 10mL methyl alcohol Phase extraction pillar is eluted, and collects eluent, and eluant, eluent nitrogen therein is blown near dry, 25 μ L of addition under water bath condition 2mg/L's13C3Atrazine-the Atrazine of mark as internal standard, then with acetonitrile and the aqueous formic acid of 0.1% mass concentration By volume 1:9 mixing, resulting solution is redissolved to residue, and it is to be measured to be settled to 1mL；
(1.3) quantitative determination：The use of HPLC-MS method to medicine is that PPCPs carries out quantitative determination；
(1.4) standard curve is drawn, is determined with inner mark method ration
(1.5) concentration and recovery of standard addition of target PPCPs pollutants in water sample to be measured are calculated
(2) determine that prediction is Predicted No Effect Concentration without effective concentration, be abbreviated as PNEC values
With aquatic organisms as biological subject, PNEC values are calculated by long-term acute toxicology data；The toxicity of use Data are learned for LC is lethal concentration, LC, inhibition concentration i.e. effective is abbreviated as Concentration, is abbreviated as the apparent inhibition concentrations of EC or non-i.e. non-observed effect concentration, contracting It is written as NOEC；
(3) calculation risk quotient is Risk Quotients, is abbreviated as RQ
Risk quotient is the concentration i.e. Measured Environmental Concentration detected in environment, is abbreviated as MEC and the ratio that prediction is PNEC without effective concentration, computing formula is RQ=MEC/PNEC；
(4) ecological risk grade is assessed
The ecological risk degree of target PPCPs compounds is estimated using risk quotient method；RQ<The chemical combination is represented when 0.01 Thing devoid of risk, 0.01≤RQ<0.1 represents that the compound has low-risk, 0.1≤RQ to environment<1 represents the compound to environment There is medium risk, RQ >=1 represents that the compound has excessive risk to environment.
2. PPCPs ecological risk evaluating methods in a kind of water environment according to claim 1, it is characterised in that the step Suddenly the HPLC-MS method that (1) (1.3) use, be using Agilent1200 liquid chromatograies- The triple level Four bar mass spectrographs of Agilent6410B determine the concentration of PPCPs, and wherein chromatographic column is Agilent ZORBAX Eclipse Plus C-18 chromatographic columns -2.1mm × 100mm, 1.8 μm；The triple mass spectrometric matter of level Four bar of Agilent6410B Spectral condition is as follows：
Ionization mode：ESI+, ion source temperature：100 DEG C, capillary voltage：4000V, EFI day with fog pressure：35.0psi.
3. PPCPs ecological risk evaluating methods in a kind of water environment according to claim 1, it is characterised in that the step Suddenly the toxicology data that (2) use is half effective concentration the 50%effective concentration, EC of inhibition concentration50。
4. PPCPs ecological risk evaluating methods in a kind of water environment according to claim 1, it is characterised in that the step Suddenly the biological subject of (2) is bacterium, algae, invertebrate or fish.
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CN107490648A (en) * 2017-09-14 2017-12-19 北京市水科学技术研究院 The assay method of medicine and personal care articles in water sample sample
CN108896670A (en) * 2018-06-19 2018-11-27 陈溪 PPCPs pollutant rapid screening detection method in Drinking Water
CN109165831A (en) * 2018-08-13 2019-01-08 中国水产科学研究院淡水渔业研究中心 Pesticide influences the methods of risk assessment of Safety of Aquatic Products in the comprehensive breeding system of rice fishing
CN109283306A (en) * 2018-09-11 2019-01-29 浙江大学 A kind of water environment endocrine disrupting evaluation method based on the response of zebra fish hormonal readiness
CN111122774A (en) * 2019-12-06 2020-05-08 国家海洋环境监测中心 Method for evaluating ecological risk safety threshold of toxic microalgae
CN111812265A (en) * 2020-07-10 2020-10-23 甘肃省药品检验研究院 Detection method for simultaneously determining 32 dyes in hair dye
CN113792983A (en) * 2021-08-20 2021-12-14 大连民族大学 Method for analyzing environmental risk of pollutants based on multidimensional evaluation factors
CN115062933A (en) * 2022-06-01 2022-09-16 生态环境部南京环境科学研究所 Multi-level risk evaluation method for microbial drug resistance of antibiotic residues in water environment

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107490648A (en) * 2017-09-14 2017-12-19 北京市水科学技术研究院 The assay method of medicine and personal care articles in water sample sample
CN108896670A (en) * 2018-06-19 2018-11-27 陈溪 PPCPs pollutant rapid screening detection method in Drinking Water
CN109165831A (en) * 2018-08-13 2019-01-08 中国水产科学研究院淡水渔业研究中心 Pesticide influences the methods of risk assessment of Safety of Aquatic Products in the comprehensive breeding system of rice fishing
CN109165831B (en) * 2018-08-13 2021-09-07 中国水产科学研究院淡水渔业研究中心 Risk assessment method for influence of pesticides on aquatic product safety in rice and fish integrated planting and breeding system
CN109283306A (en) * 2018-09-11 2019-01-29 浙江大学 A kind of water environment endocrine disrupting evaluation method based on the response of zebra fish hormonal readiness
CN111122774A (en) * 2019-12-06 2020-05-08 国家海洋环境监测中心 Method for evaluating ecological risk safety threshold of toxic microalgae
CN111812265A (en) * 2020-07-10 2020-10-23 甘肃省药品检验研究院 Detection method for simultaneously determining 32 dyes in hair dye
CN113792983A (en) * 2021-08-20 2021-12-14 大连民族大学 Method for analyzing environmental risk of pollutants based on multidimensional evaluation factors
CN115062933A (en) * 2022-06-01 2022-09-16 生态环境部南京环境科学研究所 Multi-level risk evaluation method for microbial drug resistance of antibiotic residues in water environment
CN115062933B (en) * 2022-06-01 2023-04-18 生态环境部南京环境科学研究所 Multi-level risk assessment method for microbial drug resistance of antibiotic residues in water environment

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Application publication date: 20170613