CN112394131A - Ecological risk evaluation method for corticoids in sediments - Google Patents
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Abstract
An ecological risk evaluation method of corticoids in sediments comprises the following steps: detecting the content of cortical hormone in sediment (1) extracting and concentrating the cortical hormone in the sediment; (2) decontamination of cortical hormone in the sediment; (3) quantitative analysis of corticoids; step two, determining the concentration of the corticoid in the pore water, namely Cpore(ii) a Step three, calculating Risk quotient Risk quantites, namely RQ; and step four, evaluating the ecological risk level, wherein the number of the corticoid pollutants which can be detected by the method can be up to 18, the detection limit is low, the detection result is accurate and reliable, the ecological risk evaluation model is used for calculating the risk quotient of the corticoid on the basis of quantitatively analyzing the content of the corticoid in the sediment, the risk level is determined, and a scientific basis is provided for pollution control and treatment of sediment corticoid chemicals.
Description
Technical Field
The invention belongs to the field of environmental science and ecological risk evaluation, and particularly relates to an ecological risk evaluation method for corticoids in sediments.
Background
With the rapid development of economy and the acceleration of urbanization process, a large amount of environmental hormone chemicals enter a water environment through the water outlet of a sewage treatment plant or are directly discharged artificially, and serious harm is caused to an ecological system and human health through food chain enrichment and amplification. Strict control of environmental hormone chemical pollution is definitely proposed in a water pollution control action plan published by the country in 2015, the investigation on the production and use conditions of the environmental hormone chemicals is completed before 2017, risks of a water source area, an agricultural product planting area and an aquatic product concentrated culture area are monitored and evaluated, measures such as elimination, limitation and substitution of the environmental hormone chemicals are implemented, and requirements are provided for control of the environmental hormone chemicals in the water environment from the national level.
Corticosteroids, a typical class of hormonal chemicals, are widely used in human and veterinary therapy and are the most widely used anti-inflammatory and immunosuppressive agents in the clinic. The corticoids can be classified into natural corticoids and synthetic corticoids according to their sources, and into glucocorticoids and mineralocorticoids according to their physiological functions. Synthetic glucocorticoids such as dexamethasone, prednisone, prednisolone, and methylprednisolone are widely used for treating inflammation such as arthritis, colitis, asthma, bronchitis, skin rash, allergy, rhinitis, and ophthalmia. The main sources of environmental corticosteroids are the excretion of human and vertebrate animals and the use and discharge of synthetic corticosteroid drugs. Municipal sewage treatment plants, livestock and poultry and aquaculture farms collecting human domestic sewage are pollution sources of environmental corticosteroids. The corticoids have high endocrine disrupting activity, and can cause damage to the immune, reproductive and immune systems of organisms at ng/L concentration level, and serious problems of reproductive damage, development defect and the like can be caused. In recent years, corticosteroids have been frequently detected in media such as municipal sewage, river water, sediments, and the like. The corticoids entering the water body will collect in the bottom sediment by sedimentation, and the sediment is considered as a conglomerate of the corticoids. Therefore, there is an urgent need to develop a sensitive, reliable and accurate quantitative method for simultaneously analyzing multiple corticoids in sediment.
Chinese patent CN108663471B discloses a method for determining the content of multiple endocrine disruptors in estuary sediments, which comprises the steps of pretreating estuary sediment samples by using alumina and diatomite, purifying by using Soxhlet extraction and solid-phase extraction to obtain enriched samples, and detecting and analyzing diclofenac, bisphenol A, 17 beta-estradiol, estrone, 17 alpha-ethinyl estradiol, 4-octylphenol, 4-nonylphenol, paminone, testosterone and progesterone in the sediments by using LC-MS/MS. This method requires a large amount of solvent and time, and corticoids are not analyzed. The matrix interference of a cortical hormone quantitative analysis method is large due to the complexity of the sediment matrix, the accuracy of an analysis result is influenced, and an analysis method for simultaneously and accurately detecting a plurality of trace cortical hormones in the sediment is deficient. Meanwhile, the ecological risk of corticoids in the sediment is unknown, and a serious challenge is brought to an environmental manager.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for evaluating the ecological risk of corticoids in sediments.
The invention adopts the following technical scheme:
an ecological risk evaluation method of corticoids in sediments comprises the following steps:
step one, detecting the content of cortical hormone in sediment
(1) Extracting and concentrating corticoids in sediments: putting the freeze-dried sediment into a glass container, adding an organic solvent for ultrasonic extraction, standing for clarification, taking supernatant, extracting for 1-3 times, and performing rotary evaporation and concentration on the extract to obtain an extract concentrated solution;
(2) decontamination of cortical hormones in sediment: preparing the extraction concentrated solution into water, adding trace methanol into the water, extracting through a solid phase extraction column, eluting the solid phase extraction column by using organic solvents with different polarities to obtain an eluent, and performing rotary evaporation, nitrogen-blowing concentration, constant volume and preservation on the eluent to obtain a sample solution to be detected;
(3) quantitative analysis of corticoids: introduction of CH by means of water containing 1 ‰ acetic acid in the mobile phase of the liquid phase3COO-In electrospray ionization negative ion mode, an adduct ion [ M + CH ] is formed3COO]-Simultaneously and quantitatively analyzing 18 corticoids in the sample liquid to be detected by utilizing a multi-reaction monitoring mode of a liquid chromatography-mass spectrometer;
step two, determining the concentration of the corticoid in the pore water, namely Cpore
Calculating the concentration of the corticoid in the pore water by using a distribution equilibrium model of the corticoid in the sediment-pore water, wherein the distribution equilibrium model is shown as formulas (1) and (2):
Koc＝0.63×Kow (2)
step three, calculating Risk quotient Risk quantites, namely RQ
Obtaining a risk quotient value of the corticoids by using a risk quotient calculation formula, wherein the risk quotient calculation formula is shown as (3):
step four, evaluating the ecological risk level
And (3) evaluating the ecological risk level of the corticoids in the sediment by using the obtained risk quotient: RQ < 0.01 indicates that the corticoid has low risk to environment; 0.01< RQ <1 indicates an intermediate risk of the corticoid to the environment; when the RQ is more than or equal to 1, the corticoid has high risk to the environment;
in the step (1), the organic solvent is a mixed solution of methanol and acetone, the volume ratio of the methanol to the acetone is (1-3) to 1, and the volume of the mixed solution is 15-20 mL; in the ultrasonic extraction, the ultrasonic frequency is 40KHz, the ultrasonic power is 600W, the temperature is 35 ℃, and the ultrasonic time is 15 min;
in the step (2), the solid phase extraction column is a Waters Oasis HLB or C18 solid phase extraction small column, before the solid phase extraction column is used, the solid phase extraction column is sequentially activated by ethyl acetate, acetonitrile, methanol and deionized water, the organic solvent with different polarities is a mixed solution of ethyl acetate, ethyl acetate and acetonitrile, the volume of the ethyl acetate is 6-10mL, the volume ratio of the ethyl acetate to the acetonitrile is 1 (1-3), and the volume of the mixed solution of the ethyl acetate and the acetonitrile is 15-20 mL;
in the step (3), the 18 cortical hormones are prednisone, prednisolone, cortisone, aldosterone, hydrocortisone, methylprednisolone, fluoromethalone, dexamethasone, betamethasone, triamcinolone, prednisolone acetate, hydrocortisone acetate, beclomethasone, flumethasone, budesonide, triamcinolone acetonide, dexamethasone acetate, and clobetasol propionate;
in the step (3), 18 corticoids in the sample solution to be detected are simultaneously quantitatively analyzed at one time in a multi-reaction monitoring mode of a liquid chromatography-mass spectrometer, and the specific parameters are as follows: high Performance Liquid Chromatography (HPLC): agilent 1260; a chromatographic column: waters Xbridge BEH C18 XP analytical column (2.1 mm. times.50 mm,2.5 μm); column temperature: 40 ℃; mobile phase: a: 1% o acetic acid in water, B: methanol; flow rate: 0.4 mL/min; the mobile phase gradients are shown in table 1; an acquisition mode: a multiple reaction monitoring mode; ion pair parameters for multiple reaction monitoring mode: prednisone is 417.2>357.1 (qualitative), 417.2>327.1 (quantitative); prednisolone is 419.3>359.2 (qualitative), 419.3>329.1 (quantitative); cortisone 419.3>359.2 (qualitative), 419.3>329.1 (quantitative); aldosterone was 419.2>330.9 (qualitative), 419.2>359.2 (quantitative); hydrocortisone is 421.3>361.2 (qualitative), 421.3>331.1 (quantitative); methylprednisolone 433.3>373.2 (qualitative), 433.3>343.1 (quantitative); the fluorometholone is 435.3>375.3 (qualitative), 435.3>355.1 (quantitative); dexamethasone was 451.2>391.3 (qualitative), 451.2>361.1 (quantitative); betamethasone is 451.2>391.3 (qualitative), 451.2>361.1 (quantitative); the triamcinolone is 453.1>363.2 (qualitative), 453.1>393.1 (quantitative); prednisolone acetate is 461.2>329.2 (qualitative), 461.2>401.1 (quantitative); hydrocortisone acetate is 463.3>216.8 (qualitative), 463.3>403.1 (quantitative); beclomethasone is 467.2>407.1 (qualitative), 467.2>377.1 (quantitative); the flumethasone is 469.3>409.1 (qualitative), 469.3>379.2 (quantitative); budesonide is 489.4>339.0 (qualitative), 489.4>357.2 (quantitative); triamcinolone acetonide 493.3>337.1 (qualitative), 493.3>375.0 (quantitative); the clobetasol propionate is 493.3>361.3 (qualitative), 493.3>433.3 (quantitative); dexamethasone acetate is 525.3>429.3 (qualitative), 525.3>465.3 (quantitative);
TABLE 1
| Time/min | Water volume percent/% with 1% acetic acid | Volume percent of methanol/%) |
| 0 | 90 | 10 |
| 0.5 | 90 | 10 |
| 1.5 | 40 | 60 |
| 4.0 | 30 | 70 |
| 7.0 | 25 | 75 |
| 8.5 | 0 | 100 |
| 10.0 | 0 | 100 |
| 10.5 | 90 | 10 |
| 13.5 | 90 | 10 |
Further, in the step (2) of the first step, the extraction concentrated solution is prepared into water, and the content of the added methanol is 1-3%.
Further, in the step (3), specific parameters of the liquid chromatography-mass spectrometer are as follows:
as can be seen from the above description of the present invention, compared with the prior art, the beneficial effects of the present invention are:
firstly, the extraction and concentration conditions of the corticoids in the sediment are optimized, the extraction efficiency of the target object is high, the extraction time is short, and the extraction solvent is less;
secondly, the interference effect of the sediment matrix is reduced by utilizing solid-phase extraction purification, the mixed solution of ethyl acetate, ethyl acetate and acetonitrile is limited to be used as eluent of a solid-phase extraction column, and interferents in the sediment extracting solution are removed to the greatest extent while cortical hormone is enriched so as to ensure the accuracy of an analysis result;
thirdly, the method can detect up to 18 cortical hormone pollutants, has low detection limit and accurate and reliable detection result, calculates the risk quotient of the cortical hormone by using an ecological risk evaluation model on the basis of quantitatively analyzing the content of the cortical hormone in the sediment, determines the risk level and provides scientific basis for pollution control and treatment of sediment cortical hormone chemicals.
Drawings
FIG. 1 is a total ion flow graph of an 18 corticoid target;
FIG. 2 is an extraction chromatogram of prednisone, prednisolone, cortisone, aldosterone, hydrocortisone, methylprednisolone, fluorometholone, dexamethasone, betamethasone, triamcinolone, prednisolone acetate, hydrocortisone acetate, beclomethasone, flumethasone, budesonide, triamcinolone acetonide, dexamethasone acetate, clobetasol propionate and corresponding internal standard;
FIG. 3 is a liquid phase process optimized for the separation of 18 corticoids.
Detailed Description
The invention is further described below by means of specific embodiments.
An ecological risk evaluation method of corticoids in sediments comprises the following steps:
step one, detecting the content of cortical hormone in sediment
(1) Extracting and concentrating corticoids in sediments: putting the freeze-dried sediment into a 25mL glass pointed-bottom centrifuge tube with a plug scale, firstly adding 120 mu L of 18 cortical hormone mixed standard with the concentration of 0.5mg/L and 100 mu L of hydrocortisone-D4 internal standard with the concentration of 1.0mg/L, then adding 20mL of methanol and acetone mixed solution with the volume ratio of 2:1, carrying out ultrasonic extraction with the ultrasonic frequency of 40KHz and the ultrasonic power of 600W at the temperature of 35 ℃ for 15min, standing and clarifying, taking supernatant, carrying out ultrasonic extraction for 3 times, carrying out rotary evaporation and concentration on extract liquor at the temperature of 30-35 ℃ to about 2mL to obtain extract concentrated liquor;
(2) decontamination of cortical hormones in sediment: preparing 2mL of extraction concentrate into 200mL of water, adding trace methanol, controlling the content of an organic solvent methanol in the water to be 1-3%, utilizing Waters Oasis HLB (hydrophile-lipophile balance) solid-phase extraction column to enrich a corticoid target in a solution, sequentially activating the solid-phase extraction column with 6mL of ethyl acetate, 6mL of acetonitrile, 6mL of methanol and 12mL of deionized water before use, controlling the flow rate to be 1-2 drops/second, blowing nitrogen for 30min after extraction to remove part of water in the extraction column, centrifuging for 5min under the condition of 5000r/min to remove the residual water in the extraction column, placing the extraction column into a dryer, sequentially eluting the dried solid-phase extraction column with 6mL of ethyl acetate, 15mL of a mixed solution of ethyl acetate and acetonitrile in a volume ratio of 1:2, evaporating eluent, blowing nitrogen for concentration, fixing the volume to 2mL, and storing the eluent in a brown sample injection vial;
(3) quantitative analysis of corticoids: the method comprises the following steps of (1) detecting and analyzing target substances prednisone, prednisolone, cortisone, aldosterone, hydrocortisone, methylprednisolone, fluoromethalone, dexamethasone, betamethasone, triamcinolone, prednisolone acetate, hydrocortisone acetate, beclomethasone, flumethasone, budesonide, triamcinolone acetonide, dexamethasone acetate and clobetasol propionate 18 corticoids based on a multi-reaction monitoring mode established by a liquid chromatography-mass spectrometer, and quantifying the corticoids by using an internal standard method, wherein the parameters are as follows:
high Performance Liquid Chromatography (HPLC): agilent 1260;
mass spectrometry: API 4000QTrap-AB SCIEX;
a chromatographic column: waters Xbridge BEH C18 XP analytical column (2.1 mm. times.50 mm,2.5 μm); column temperature: 40 ℃;
mobile phase: a: 1% o acetic acid in water, B: methanol; flow rate: 0.4 mL/min; the sample injection volume is 10 mu L;
mobile phase gradiometer, as follows:
TABLE 1
The specific parameters of the liquid chromatography-mass spectrometer are as follows:
TABLE 2
The parameters for quantitative analysis of corticoids using the multiple response monitoring model are shown in Table 3
TABLE 3
Step two, determining the concentration of the corticoid in the pore water, namely Cpore
Calculating the concentration of the corticoid in the pore water by using a distribution equilibrium model of the corticoid in the sediment-pore water, wherein the distribution equilibrium model is shown as formulas (1) and (2):
Koc＝0.63×Kow (2)
wherein, Cpore: the concentration of pollutants in pore water, ng/L; csed: concentration of contaminants in the sediment, ng/g; f. ofoc: the total organic carbon content in the sediment is g/kg; koc: the distribution coefficient of pollutants in sediment-pore water is L/kg; kow: the n-octanol-water partition coefficient of the contaminant;
step three, calculating Risk quotient Risk quantites, namely RQ
Obtaining a risk quotient value of the corticoids by using a risk quotient calculation formula, wherein the risk quotient calculation formula is shown as (3):
wherein, PNEC: predicting the ineffective response concentration; RQ: a risk quotient;
step four, evaluating the ecological risk level
And (3) evaluating the ecological risk level of the corticoids in the sediment by using the obtained risk quotient: RQ < 0.01 indicates that the corticoid has low risk to environment; 0.01< RQ <1 indicates an intermediate risk of the corticoid to the environment; RQ ≧ 1 indicates that the corticosteroid presents a high risk to the environment.
Specifically, regarding the predicted non-effect concentration PENC, the european union risk Assessment technical guideline uses an evaluation factor (AF) method to derive the predicted non-effect concentration PNEC, and table 4 gives the selection principle of the evaluation factor used for deriving the PNEC. For the first case, PNEC were at half lethal (effective) concentrations L (E) C50To the corresponding evaluation factor AF. For the second to fourth cases, PNEC is the ratio of the minimum of the maximum observed no-effect concentrations NOEC to the corresponding evaluation factor AF. For the fifth case, the SSD curve of the species sensitivity distribution was obtained with the chronic toxicity data of the contaminant versus the abscissa and the cumulative probability of effect as the ordinate. SSD curve fitting is usually done using Log-normal or Log-logistic models, and then its rationality is judged by either the K-S test (Kolmogorov-Smirnov test) or the A-D goodness of fit test (Anderson-Darling goodness of fit test). Finally, the concentration corresponding to the SSD curve 5% probability (HC5 value) was divided by AF to derive PNEC and the 50% confidence interval associated with that concentration was taken (c.i.), as shown in equation (4). The PNEC values of prednisolone, cortisone, hydrocortisone, dexamethasone are shown in table 5.
Table 4 deduces the evaluation factor (AF) values required for PNEC:
TABLE 5
The method has the advantages that the number of corticoid pollutants which can be detected is up to 18, the detection limit is low, the detection result is accurate and reliable, the risk quotient of the corticoid is calculated by using an ecological risk evaluation model on the basis of quantitatively analyzing the content of the corticoid in the sediment, the risk grade is determined, scientific basis is provided for pollution control and treatment of sediment corticoid chemicals, the sediment matrix interference effect is reduced by adopting solid-phase extraction and purification, the mixed solution of ethyl acetate, ethyl acetate and acetonitrile is limited to be used as eluent of a solid-phase extraction column, and the interferent in the sediment extracting solution is removed to the greatest extent while the corticoid is enriched so as to ensure the accuracy of the analysis result.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims and their equivalents and modifications within the scope of the description.
Claims (3)
1. An ecological risk evaluation method of corticoids in sediments is characterized in that: the method comprises the following steps:
step one, detecting the content of cortical hormone in sediment
(1) Extracting and concentrating corticoids in sediments: putting the freeze-dried sediment into a glass container, adding an organic solvent for ultrasonic extraction, standing for clarification, taking supernatant, extracting for 1-3 times, and performing rotary evaporation and concentration on the extract to obtain an extract concentrated solution;
(2) decontamination of cortical hormones in sediment: preparing the extraction concentrated solution into water, adding trace methanol into the water, extracting through a solid phase extraction column, eluting the solid phase extraction column by using organic solvents with different polarities to obtain an eluent, and performing rotary evaporation, nitrogen-blowing concentration, constant volume and preservation on the eluent to obtain a sample solution to be detected;
(3) quantitative analysis of corticoids: introduction of CH by means of water containing 1 ‰ acetic acid in the mobile phase of the liquid phase3COO-In electrospray ionization negative ion mode, an adduct ion [ M + CH ] is formed3COO]-Simultaneously and quantitatively analyzing 18 corticoids in the sample liquid to be detected by utilizing a multi-reaction monitoring mode of a liquid chromatography-mass spectrometer;
step two, determining the concentration of the corticoid in the pore water, namely Cpore
Calculating the concentration of the corticoid in the pore water by using a distribution equilibrium model of the corticoid in the sediment-pore water, wherein the distribution equilibrium model is shown as formulas (1) and (2):
Koc＝0.63×Kow (2)
step three, calculating Risk quotient Risk quantites, namely RQ
Obtaining a risk quotient value of the corticoids by using a risk quotient calculation formula, wherein the risk quotient calculation formula is shown as (3):
step four, evaluating the ecological risk level
And (3) evaluating the ecological risk level of the corticoids in the sediment by using the obtained risk quotient: RQ < 0.01 indicates that the corticoid has low risk to environment; 0.01< RQ <1 indicates an intermediate risk of the corticoid to the environment; when the RQ is more than or equal to 1, the corticoid has high risk to the environment;
in the step (1), the organic solvent is a mixed solution of methanol and acetone, the volume ratio of the methanol to the acetone is (1-3) to 1, and the volume of the mixed solution is 15-20 mL; in the ultrasonic extraction, the ultrasonic frequency is 40KHz, the ultrasonic power is 600W, the temperature is 35 ℃, and the ultrasonic time is 15 min;
in the step (2), the solid phase extraction column is a Waters Oasis HLB or C18 solid phase extraction small column, before the solid phase extraction column is used, the solid phase extraction column is sequentially activated by ethyl acetate, acetonitrile, methanol and deionized water, the organic solvent with different polarities is a mixed solution of ethyl acetate, ethyl acetate and acetonitrile, the volume of the ethyl acetate is 6-10mL, the volume ratio of the ethyl acetate to the acetonitrile is 1 (1-3), and the volume of the mixed solution of the ethyl acetate and the acetonitrile is 15-20 mL;
in the step (3), the 18 cortical hormones are prednisone, prednisolone, cortisone, aldosterone, hydrocortisone, methylprednisolone, fluoromethalone, dexamethasone, betamethasone, triamcinolone, prednisolone acetate, hydrocortisone acetate, beclomethasone, flumethasone, budesonide, triamcinolone acetonide, dexamethasone acetate, and clobetasol propionate;
in the step (3), 18 corticoids in the sample solution to be detected are simultaneously quantitatively analyzed at one time in a multi-reaction monitoring mode of a liquid chromatography-mass spectrometer, and the specific parameters are as follows: high Performance Liquid Chromatography (HPLC): agilent 1260; a chromatographic column: waters Xbridge BEH C18 XP analytical column (2.1 mm. times.50 mm,2.5 μm); column temperature: 40 ℃; mobile phase: a: 1% o acetic acid in water, B: methanol; flow rate: 0.4 mL/min; the mobile phase gradients are shown in table 1; an acquisition mode: a multiple reaction monitoring mode; ion pair parameters for multiple reaction monitoring mode: prednisone is 417.2>357.1 (qualitative), 417.2>327.1 (quantitative); prednisolone is 419.3>359.2 (qualitative), 419.3>329.1 (quantitative); cortisone 419.3>359.2 (qualitative), 419.3>329.1 (quantitative); aldosterone was 419.2>330.9 (qualitative), 419.2>359.2 (quantitative); hydrocortisone is 421.3>361.2 (qualitative), 421.3>331.1 (quantitative); methylprednisolone 433.3>373.2 (qualitative), 433.3>343.1 (quantitative); the fluorometholone is 435.3>375.3 (qualitative), 435.3>355.1 (quantitative); dexamethasone was 451.2>391.3 (qualitative), 451.2>361.1 (quantitative); betamethasone is 451.2>391.3 (qualitative), 451.2>361.1 (quantitative); the triamcinolone is 453.1>363.2 (qualitative), 453.1>393.1 (quantitative); prednisolone acetate is 461.2>329.2 (qualitative), 461.2>401.1 (quantitative); hydrocortisone acetate is 463.3>216.8 (qualitative), 463.3>403.1 (quantitative); beclomethasone is 467.2>407.1 (qualitative), 467.2>377.1 (quantitative); the flumethasone is 469.3>409.1 (qualitative), 469.3>379.2 (quantitative); budesonide is 489.4>339.0 (qualitative), 489.4>357.2 (quantitative); triamcinolone acetonide 493.3>337.1 (qualitative), 493.3>375.0 (quantitative); the clobetasol propionate is 493.3>361.3 (qualitative), 493.3>433.3 (quantitative); dexamethasone acetate is 525.3>429.3 (qualitative), 525.3>465.3 (quantitative);
TABLE 1
。
2. The method for ecological risk assessment of corticoids in sediments as claimed in claim 1, wherein: in the step (2), the extraction concentrated solution is prepared into water, and the content of the added methanol is 1-3%.
3. The method for ecological risk assessment of corticoids in sediments as claimed in claim 1, wherein: in the step (3), the specific parameters of the liquid chromatography-mass spectrometer are as follows:
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