CN109813818A - A kind of detection method of water quality content of phenolic compounds - Google Patents
A kind of detection method of water quality content of phenolic compounds Download PDFInfo
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- CN109813818A CN109813818A CN201910087899.8A CN201910087899A CN109813818A CN 109813818 A CN109813818 A CN 109813818A CN 201910087899 A CN201910087899 A CN 201910087899A CN 109813818 A CN109813818 A CN 109813818A
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Abstract
The present invention relates to a kind of detection methods of water quality content of phenolic compounds, and described method includes following steps: (1) extracting sample liquid to be derived；(2) derivatization of sample: the derivative agent of 100 μ L first is added in sample liquid to be derived and is placed in GC-MS and tests and analyzes after reacting 1h at room temperature, first derivatization reagent is BSTFA；(3) derivatization of standard working solution；(4) concentration is calculated.The step of embodiment of the present invention is by changing to derivatization sample liquid and derivatization reagent, it is simpler compared in national standard so that appearance better effect, and in derivatization without carrying out heating replacement solvent, and derivatization reagent price used is cheaper, cost performance is higher.
Description
Technical field
The present invention relates to water quality inspection technique field, in particular to a kind of detection method of water quality content of phenolic compounds.
Background technique
The phenol wastewater of the mainly some industrial enterprise's discharges of phenol pollution in water body, such as coking, papermaking, plastics, dye
Many industry such as material, drug, herbicide, pesticide, timber processing, when the concentration of phenol in water body reaches 0.1-0.2mg/L,
Phenol will be contained in the fish body lived in this water body, if people has eaten this fish, the phenol amount for taking in body is more than the solution of human body
When malicious ability, slow poisoning will occur, the symptoms such as headache, dizziness, vomiting, diarrhea, neurological disorders, anaemia occur, with pollution
The water crossed forms chlorophenol as drinking water under the action of disinfection chlorine, and taste is reinforced one to two orders of magnitude and produces
Raw stench, and phenolic compound has the genotoxic potential of carcinogenic mutagenicity, therefore the discharge of phenol is by strict regulations.
The detection that gas chromatography-mass spectrography carries out content of phenolic compounds is generallyd use at present, and according to spreading out in national standard
Biochemical reagents handle sample, then appearance effect is poor after being detected by gas chromatograph-mass spectrometer, even without
Peak occurs.
Summary of the invention
In order to solve the above technical problems, having the present invention provides a kind of detection method of water quality content of phenolic compounds
The good advantage of appearance effect.
In order to achieve the above objectives, technical scheme is as follows:
A kind of detection method of water quality content of phenolic compounds, described method includes following steps:
(1) sample liquid to be derived is extracted
It takes 500ml water sample to be measured to be placed in 1L separatory funnel, sulfuric acid is added and adjusts water sample pH≤1, weighs 15g sodium chloride and arrives
In water sample to be measured, shaking is dissolved, measurement 50ml dichloromethane-ethyl acetate mixed solution, after shaking out 10min, is stood and is received
Collect organic phase, and is removed water through anhydrous sodium sulfate；
Above-mentioned extraction step in triplicate, combining extraction liquid is close dry through Rotary Evaporators concentration, is settled to n-hexane
1ml obtains sample liquid to be derived；
(2) derivatization of sample
100 the first derivatization reagents of μ L are added in sample liquid to be derived, after reacting 1h at room temperature, is placed in GC-MS and detects
Analysis, first derivatization reagent are BSTFA；
(3) derivatization of standard working solution
With n-hexane make solvent configuration phenolic compound concentration be 0.1mg/L, 0.2mg/L, 0.4mg/L, 1.0mg/L,
The standard working solution of 2.4mg/L is separately added into 100 the second derivatization reagents of μ L, after reacting 1h at room temperature, is placed in GC-MS
It tests and analyzes, second derivatization reagent is the reagent that volume ratio is BSTFA:TMCS=99:1；
(4) concentration is calculated
Standard curve is established according to the analysis result of standard working solution, the standard curve is to sit with peak area is vertical
The one-variable linear regression of formation is drawn in mark, the conventional coordinates established using the concentration of corresponding phenolic compound as abscissa
The relation curve of peak area and concentration；
The phenolic compound obtained in sample liquid to be derived according to the analysis result establishing criteria curve of sample liquid to be derived is dense
It spends, and the content of phenolic compound is calculated according to calibration curve equation.
As a preferred solution of the present invention, when GC-MS is tested and analyzed, the column temperature of chromatographic column is according to following mistake
Cheng Bianhua: 40 DEG C of holding 2min of initial temperature, then risen to after 120 DEG C with 10 DEG C/min and keep 1min, then risen to 25 DEG C/min
2min is kept after 250 DEG C, then rises to 290 DEG C with 10 DEG C/min.
As a preferred solution of the present invention, the calibration curve equation are as follows: R=C × V/500；Wherein,
R is content of phenolic compounds in sample liquid to be derived；
C is the concentration of phenolic compound in the sample liquid obtained by standard curve；
V is sample liquid constant volume to be derived；
500 be volume of water sample to be measured.
In conclusion the invention has the following beneficial effects:
The step of embodiment of the present invention is by changing to derivatization sample liquid and derivatization reagent, so that appearance better effect,
And in derivatization without carrying out heating replacement solvent, derivatization examination simpler compared in national standard and used
Agent price is cheaper, and cost performance is higher.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
Logical technical staff every other embodiment obtained without creative efforts, belongs to protection of the present invention
Range.
Embodiment
A kind of detection method of water quality content of phenolic compounds, described method includes following steps:
(1) sample liquid to be derived is extracted
It takes 500ml water sample to be measured to be placed in 1L separatory funnel, sulfuric acid is added and adjusts water sample pH≤1, weighs 15g sodium chloride and arrives
In water sample to be measured, shaking is dissolved, measurement 50ml dichloromethane-ethyl acetate mixed solution, after shaking out 10min, is stood and is received
Collect organic phase, and is removed water through anhydrous sodium sulfate；
Above-mentioned extraction step in triplicate, combining extraction liquid is close dry through Rotary Evaporators concentration, is settled to n-hexane
1ml obtains sample liquid to be derived.
(2) derivatization of sample
100 the first derivatization reagents of μ L are added in sample liquid to be derived, after reacting 1h at room temperature, is placed in GC-MS and detects
Analysis, first derivatization reagent are BSTFA.
GC-MS (Gas Chromatography-Mass Spectrometer) refers to gas chromatograph-mass spectrometer (GC-MS),
When GC-MS is tested and analyzed, the column temperature of chromatographic column changes according to following procedure: 40 DEG C of holding 2min of initial temperature, then with
10 DEG C/min keeps 1min after rising to 120 DEG C, then is risen to after 250 DEG C with 25 DEG C/min and keep 2min, then is risen to 10 DEG C/min
290℃。
The specification of the chromatographic column of GC-MS is 30m × 0.25mm × 0.25 μm, and injector temperature is set as 280 DEG C, ion
Source temperature is set as 200 DEG C, and interface temperature is 280 DEG C, flow control 1.0mL/min, and sample volume is 1 μ L, and input mode is
Splitless injecting samples, detection pattern select full scan mode.
(3) derivatization of standard working solution
With n-hexane make solvent configuration phenolic compound concentration be 0.1mg/L, 0.2mg/L, 0.4mg/L, 1.0mg/L,
The standard working solution of 2.4mg/L is separately added into 100 the second derivatization reagents of μ L, after reacting 1h at room temperature, is placed in GC-MS
It tests and analyzes, second derivatization reagent is the reagent that volume ratio is BSTFA:TMCS=99:1；The wherein work of GC-MS
It is required that identical with step (2).
(4) concentration is calculated
Standard curve is established according to the analysis result of standard working solution, the standard curve is to sit with peak area is vertical
The one-variable linear regression of formation is drawn in mark, the conventional coordinates established using the concentration of corresponding phenolic compound as abscissa
The relation curve of peak area and concentration；
The phenolic compound obtained in sample liquid to be derived according to the analysis result establishing criteria curve of sample liquid to be derived is dense
It spends, and the content of phenolic compound is calculated according to calibration curve equation.
Calibration curve equation are as follows: R=C × V/500；Wherein,
R is content of phenolic compounds in sample liquid to be derived, and unit is micro- gram per liter (μ g/L)；
C is the concentration of phenolic compound in the sample liquid obtained by standard curve, and unit is micrograms per millilitre (μ g/mL)；
V is sample liquid constant volume to be derived, and unit is milliliter (mL)；
500 be volume of water sample to be measured, and unit is milliliter (mL).
The step of embodiment of the present invention is by changing to derivatization sample liquid and derivatization reagent, so that appearance better effect,
And in derivatization without carrying out heating replacement solvent, derivatization examination simpler compared in national standard and used
Agent price is cheaper, and cost performance is higher.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, defined herein
General Principle can realize in other embodiments without departing from the spirit or scope of the present invention.Therefore, originally
Invention is not intended to be limited to the embodiments shown herein, and is to fit to special with principles disclosed herein and novelty
The consistent widest scope of point.
Claims (3)
1. a kind of detection method of water quality content of phenolic compounds, which is characterized in that described method includes following steps:
(1) sample liquid to be derived is extracted
It takes 500ml water sample to be measured to be placed in 1L separatory funnel, sulfuric acid is added and adjusts water sample pH≤1, weighs 15g sodium chloride to water to be measured
In sample, shaking is dissolved, measurement 50ml dichloromethane-ethyl acetate mixed solution, and after shaking out 10min, it is organic to stand collection
Phase, and removed water through anhydrous sodium sulfate；
Above-mentioned extraction step in triplicate, combining extraction liquid is close dry through Rotary Evaporators concentration, is settled to 1ml with n-hexane and obtains
Sample liquid to be derived；
(2) derivatization of sample
100 the first derivatization reagents of μ L are added in sample liquid to be derived, after reacting 1h at room temperature, is placed in GC-MS and tests and analyzes,
First derivatization reagent is BSTFA；
(3) derivatization of standard working solution
Make solvent configuration phenolic compound concentration with n-hexane as 0.1mg/L, 0.2mg/L, 0.4mg/L, 1.0mg/L, 2.4mg/L
Standard working solution, be separately added into 100 the second derivatization reagents of μ L, after reacting 1h at room temperature, be placed in GC-MS detection point
Analysis, second derivatization reagent is the reagent that volume ratio is BSTFA:TMCS=99:1；
(4) concentration is calculated
Establish standard curve according to the analysis result of standard working solution, the standard curve be with peak area ordinate, with
The one-variable linear regression peak area of formation is drawn in the conventional coordinates that the concentration of corresponding phenolic compound is established for abscissa
With the relation curve of concentration；
The phenolic compound concentration in sample liquid to be derived, and root are obtained according to the analysis result establishing criteria curve of sample liquid to be derived
The content of phenolic compound is calculated according to calibration curve equation.
2. the detection method of water quality content of phenolic compounds according to claim 1, which is characterized in that GC-MS is examined
When surveying analysis, the column temperature of chromatographic column changes according to following procedure: 40 DEG C of holding 2min of initial temperature, then is risen to 10 DEG C/min
1min is kept after 120 DEG C, then is risen to after 250 DEG C with 25 DEG C/min and keeps 2min, then rises to 290 DEG C with 10 DEG C/min.
3. the detection method of water quality content of phenolic compounds according to claim 2, which is characterized in that the standard curve
Equation are as follows: R=C × V/500；Wherein,
R is content of phenolic compounds in sample liquid to be derived；
C is the concentration of phenolic compound in the sample liquid obtained by standard curve；
V is sample liquid constant volume to be derived；
500 be volume of water sample to be measured.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731557A (en) * | 2011-04-02 | 2012-10-17 | 北京市理化分析测试中心 | Steroid substance derivation method and its analysis detection method |
| CN102841161A (en) * | 2012-09-27 | 2012-12-26 | 浙江省海洋水产研究所 | Gas chromatography-mass spectrometric detection method for octyl phenol and nonyl phenol in aquatic products |
| CN104914202A (en) * | 2015-05-06 | 2015-09-16 | 宁波市海洋与渔业研究院 | Method for determining sediment and 19 chlorophenols in soil by gas chromatography-mass spectrography |
| CN104977382A (en) * | 2015-06-13 | 2015-10-14 | 西南科技大学 | Analysis method for simultaneously determining tiny amounts of 6 phenolic endocrine disrupting chemicals in water environment |
-
2019
- 2019-01-29 CN CN201910087899.8A patent/CN109813818A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731557A (en) * | 2011-04-02 | 2012-10-17 | 北京市理化分析测试中心 | Steroid substance derivation method and its analysis detection method |
| CN102841161A (en) * | 2012-09-27 | 2012-12-26 | 浙江省海洋水产研究所 | Gas chromatography-mass spectrometric detection method for octyl phenol and nonyl phenol in aquatic products |
| CN104914202A (en) * | 2015-05-06 | 2015-09-16 | 宁波市海洋与渔业研究院 | Method for determining sediment and 19 chlorophenols in soil by gas chromatography-mass spectrography |
| CN104977382A (en) * | 2015-06-13 | 2015-10-14 | 西南科技大学 | Analysis method for simultaneously determining tiny amounts of 6 phenolic endocrine disrupting chemicals in water environment |
Non-Patent Citations (3)
| Title |
|---|
| DONGHAO LI 等: "Silyl Derivatization of Alkylphenols, Chlorophenols,and Bisphenol A for Simultaneous GC/MS Determination", 《ANAL. CHEM.》 * |
| 朱丽波 等: "水体中酚类化合物分析方法的比较研究", 《中国环境监测》 * |
| 熊丽蓓 等: "水中双酚A 和烷基酚聚氧乙烯醚降解物的GC-MS测定方法研究", 《环境卫生学杂志》 * |
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Application publication date: 20190528 |