CN111398435A - Solid phase extraction-gas chromatography-mass spectrometry method for simultaneously detecting multiple trace free amino acids in water source - Google Patents
Solid phase extraction-gas chromatography-mass spectrometry method for simultaneously detecting multiple trace free amino acids in water source Download PDFInfo
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- 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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- G—PHYSICS
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Abstract
The invention provides a solid phase extraction-gas chromatography-mass spectrometry method for simultaneously detecting various trace free amino acids in a water source. The method comprises the following steps: collecting a water sample, purifying and enriching the water sample, performing esterification derivatization treatment to obtain a sample solution, performing GC-MS detection on the sample solution, and measuring the peak area and the peak emergence time of the characteristic ions of the amino acid derivatives in the sample solution; preparing amino acid mixed standard stock solutions with different concentrations, performing esterification and derivatization treatment respectively, performing GC-MS detection respectively, detecting the peak surface of characteristic ions of amino acid derivatives in the sample stock solutions, and performing a linear regression equation on the peak surface according to the mass concentration of the solutions to obtain the linear regression equation of the amino acids; and calculating the content of the amino acid in the sample solution by using a linear regression equation of the amino acid. The invention solves the problems of complex water quality and components in the water source water and high difficulty in amino acid detection, and improves the accuracy, stability and reliability of amino acid detection.
Description
Technical Field
The invention relates to the field of water quality detection, in particular to a method for simultaneously detecting various trace free amino acids in a water source.
Technical Field
The amino acid is the most basic substance related to life activities, is the most basic unit for constituting protein, and is the most common natural nitrogen-containing organic matter with large proportion in water sources, the concentration of the amino acid in the soluble organic nitrogen in the surface water is up to 15-35%, and the concentration of the amino acid detected in the surface river water is 100-500 mu g/L in natural water bodies.
Most amino acids are hydrophilic substances and are difficult to remove in the conventional water treatment process, the amino acids have high chlorine demand, and in the chlorination disinfection process, on one hand, the chlorine consumption is increased, and on the other hand, more carbon-containing disinfection byproducts and nitrogen-containing disinfection byproducts are generated, so that the amino acids are typical precursors of the nitrogen-containing disinfection byproducts. In addition, amino acids may also serve as potential carbon and nitrogen sources to promote the growth of microorganisms in the pipe network.
The content of amino acid in the water source water is directly related to factors such as water type, algae content, season change and the like, so that the content detection of the amino acid as a nitrogen-containing precursor in the water source environment has important significance from the aspect of controlling disinfection byproducts.
Spackman et al, for the first time, use post-column ninhydrin derivatization in combination with ion exchange chromatography to analyze amino acids generated by proteolysis, and lay the foundation of modern automatic amino acid analysis techniques. With the continuous development of detection technology, new amino acid analysis methods are continuously discovered, common amino acid detection methods comprise ion exchange chromatography, high performance liquid chromatography, liquid chromatography-mass spectrometry, capillary electrophoresis and the like, various detection methods have advantages and disadvantages, the ion exchange chromatography can only carry out derivatization on primary amino acid, and a heating derivatization device is required. The liquid chromatography-mass spectrometry is simple and rapid, can realize qualitative and quantitative analysis at the same time, but has expensive instruments and equipment. The capillary electrophoresis method is time-consuming, labor-consuming and has poor reproducibility in amino acid analysis.
Disclosure of Invention
The invention aims to solve the technical problems, adopts solid-phase extraction combined with gas detection to analyze amino acid, has good sensitivity and accuracy, high reliability and more general instruments and equipment, is more suitable for measuring trace amino acid in water environment, provides a method for simultaneously detecting multiple trace free amino acids in a water source, solves the problems of complex water quality components in the water source water and higher amino acid detection difficulty, and improves the accuracy, stability and reliability of amino acid detection.
The technical scheme adopted by the invention for solving the technical problems is as follows: a solid phase extraction-gas chromatography-mass spectrometry method for simultaneously detecting various trace free amino acids in a water source comprises the following steps:
s1, collecting a water sample;
s2, purifying and enriching the water sample in the S1, and obtaining the purified and enriched water sample by adopting a solid phase extraction mode;
s3, performing esterification derivatization treatment on the water sample treated in the S2 to obtain a sample solution;
s4, detecting the sample solution obtained in the S3 by adopting GC-MS, and measuring the peak area and the peak emergence time of the characteristic ions of the amino acid derivatives in the sample solution;
s5, preparing amino acid mixed standard stock solutions, sequentially carrying out S3 operations on the amino acid mixed standard stock solutions with different solution mass concentrations to obtain sample stock solutions, carrying out GC-MS detection on the sample stock solutions respectively, detecting peak surfaces of characteristic ions of amino acid derivatives in the sample stock solutions, and carrying out a linear regression equation on the peak surfaces according to the solution mass concentrations to obtain a linear regression equation of the amino acids;
and S6, according to the amino acid linear regression equation in S5, calculating the content of the amino acid in the peak area and the peak emergence time of the characteristic ion of the amino acid derivative measured in S4.
Preferably, the solid phase extraction in S2 comprises the following steps,
step 1, adjusting the pH value of a water sample to 1.3 by using hydrochloric acid before loading the water sample on a column, and rinsing the activated column by using 4.5m L methanol and 9m L hydrochloric acid;
step 2, passing the water sample through the column at the speed of 2m L/min, and then eluting by taking 9m L methanol solution containing 5% ammonia water for three times, wherein 3m L is used for elution each time to obtain eluent;
and 3, drying the eluent by using a nitrogen blowing instrument, and dissolving the eluent by using hydrochloric acid with the concentration of 1m L to finally obtain a purified and enriched water sample.
Preferably, the concentration of the hydrochloric acid is 0.1 mol/L.
Preferably, the treatment of esterification derivatization in S3 includes the following steps;
step 1, taking 100 mu L of water sample purified and enriched in S2 to a reaction tube, adding 50 mu L of dichloromethane, blowing the water sample to a nitrogen blowing instrument for drying, adding 50 mu L of hydrochloric acid-n-butanol, and putting the mixture into a 120 ℃ oven for esterification for 60min to obtain a sample A;
step 2, adding 50 mu L dichloromethane, 100 mu L ethyl acetate and 100 mu L trifluoroacetic anhydride into the sample A, and sealing the tube to obtain a sample B;
and step 3: placing the reaction tube provided with the sample B into an oven for acylation at 120 ℃ for 30 min;
and 4, blowing the acylated sample B by using a nitrogen blowing instrument, and adding 500 mu L of dichloromethane for dissolution to obtain a sample solution.
Preferably, the concentration of the hydrochloric acid-n-butanol is 3.5 mol/L.
Preferably, the GC-MS detection comprises the following conditions that the temperature of a vaporization chamber is 280 ℃, the carrier gas is high-purity He, the flow rate is 1.0m L/min, the ionization energy of an EI source is 70ev, the temperature is 200 ℃, the filament current is 220mA, the interface temperature is 250 ℃, the temperature of a chromatographic column is 70-300 ℃, the retention time is 2-15 min, the heating rate is 15 ℃/min, the qualitative is carried out by using a full scanning mode, the mass scanning range is 40-600amu, the quantitative is carried out by using an SIM mode, and the ion scanning m/z is selected to be alanine 140, threonine 153, serine 139, valine 168, leucine 182, isoleucine 82, proline 166, aspartic acid 240, phenylalanine 91 and glutamic acid 180.
Preferably, the amino acid mixed standard stock solution in S5 is prepared by mixing different kinds of amino acid stock solutions, and the preparation of the amino acid stock solution comprises the following steps of weighing amino acid solids and preparing 50m L stock solution by using 0.1 mol/L HCl.
Preferably, the amino acid solids include alanine, threonine, serine, valine, leucine, isoleucine, proline, aspartic acid, phenylalanine, and glutamic acid.
Preferably, the solution mass concentration of the amino acid mixed standard stock solution comprises 0.1, 0.5, 1, 2, 5, 10, 20 and 30 mg/L.
Preferably, the linear regression equation in S5 is used to perform linear regression analysis with the peak area of the characteristic ion of the amino acid derivative as the Y-axis and the concentration as the X-axis.
The method has the beneficial effects that the content of 10 trace free amino acids in a water source can be detected simultaneously by the amino acid detection method, the detection limit of the 10 amino acids in the method is 2.3-13.9 mu g/L, the reliability of solid phase extraction and derivatization is verified by a labeling recovery test, and the recovery rate is about 80%.
Enriching a sample by adopting a solid phase extraction column with strong cation exchange SCX filler; taking the enriched water sample for derivatization treatment, and derivatizing the free amino acid with strong polarity, poor thermal stability and strong chemical activity into amino acid ester with weak polarity, easy volatilization and good thermal stability; and then, testing and analyzing the sample by using a gas chromatography-mass spectrometer, in order to avoid the reduction of analysis sensitivity caused by impurities generated in the derivatization process, determining the amino acid in the sample by using a full-scan mode, and quantifying by using a Selected Ion Mode (SIM). The method can realize the simultaneous detection of various trace free amino acids in water sources, and has the advantages of accuracy, reliability, high sensitivity, high efficiency, good repeatability and stability and the like.
The invention utilizes strong cation exchange material to carry out solid phase extraction enrichment pretreatment on actual water sample, can effectively remove impurities in some matrixes and improve the recovery rate. Meanwhile, the gas chromatography-mass spectrometry combined method is adopted for detection, and through selection of different amino acid characteristic ions, the influence of interference peak values is effectively avoided, and the detection sensitivity and accuracy are improved.
Drawings
FIG. 1: the chromatogram map of the 10 amino acid standard substance derivatives is shown;
FIG. 2: is a graph of the normalized recovery of the amino acid of the invention in pure water;
FIG. 3: is a graph of the recovery of the amino acid of the invention in tap water with a standard;
FIG. 4: the recovery rate of the amino acid in raw water is shown in the figure.
Detailed Description
The invention provides a solid phase extraction-gas chromatography-mass spectrometry method for simultaneously detecting various trace free amino acids in a water source, and in order to make the purposes, technical schemes and advantages of the invention more clear, the invention is further described in detail by combining specific examples below, which should not be construed as limiting the invention.
The following are examples: simultaneously measuring the content of 10 trace free amino acids in a water source
A solid phase extraction-gas chromatography-mass spectrometry method for simultaneously detecting various trace free amino acids in a water source comprises the following steps:
the method comprises the following steps of S1, water sample collection, 3 times of collection of source water, process effluent water of a water plant and factory water for amino acid detection in the period of 12 months to 5 months in 2017, wherein a CX water plant in H market takes DT stream and L HT reservoirs as water sources, a TH water plant takes water from T lake, the CX water plant adopts a traditional conventional treatment process, and the TH water plant adopts an advanced treatment process of ozone oxidation and activated carbon.
The water sample is taken and immediately taken back to the laboratory, filtered by a 0.45 mu m filter membrane and stored in a brown bottle and stored in a shading environment at 4 ℃.
S2, purifying and enriching a water sample in S1, obtaining the purified and enriched water sample by adopting a solid phase extraction mode, pretreating the water sample, enriching a 1L water sample by solid phase extraction (a solid phase extraction column adopts strong cation exchange SCX packing), adjusting the pH value of the water sample to 1.3 by hydrochloric acid before being loaded on the column, rinsing the activated column by 4.5m L methanol and 9m L0.1.0.1 mol/L hydrochloric acid, passing the water sample through the column at the speed of 2m L/min, then taking 9m L methanol solution containing 5% ammonia water for three times for elution, carrying out elution by 3m L each time, blowing the water sample by a nitrogen blower after the elution is finished, and dissolving the water sample by 1m L0.1.0.1 mol/L hydrochloric acid for later use.
S3, performing esterification and derivatization treatment on the water sample treated in the S2 to obtain a sample solution, performing derivatization treatment on the enriched water sample 100 mu L, adding 50 mu L dichloromethane, drying by using a nitrogen blower, adding hydrochloric acid-n-butyl alcohol with the concentration of 50 mu L being 3.5 mol/L, putting the water sample into a 120 ℃ oven for esterification for 60min to obtain a sample A, adding 50 mu L dichloromethane, 100 mu L ethyl acetate and 100 mu L trifluoroacetic anhydride, sealing the tube to obtain a sample B, putting the reaction tube provided with the sample B into the oven for acylation at 120 ℃ for 30min, drying by using a nitrogen blower, and adding 500 mu L dichloromethane for dissolution to obtain the sample solution.
And S4, detecting the sample solution obtained in S3 by adopting GC-MS, and measuring the peak area and the peak emergence time of characteristic ions of amino acid derivatives in the sample solution, wherein the qualitative and quantitative analysis of free amino acids depends on the retention time and the area of peaks of the derivatives, the detection of the GC-MS comprises the following conditions that the temperature of a vaporization chamber is 280 ℃, the carrier gas is high-purity He, the flow rate is 1.0m L/min, the ionization energy of an EI source is 70ev, the temperature is 200 ℃, the filament current is 220mA, the interface temperature is 250 ℃, the temperature of a chromatographic column is 70-300 ℃, the retention time is 2-15 min, the heating speed is 15 ℃/min, the sample solution is characterized by using a full scan mode, the mass scan range is 40-600amu, and the sample solution is quantified by using a SIM mode, the ion scan m/z is alanine (Ala)140, Thr)153, serine (Ser)139, valine (Val)168, leucine (L eu)182, isoleucine (I L e)182, proline (Pro)166, aspartic acid (Asp)240, and glutamic acid (Glu) 180.
The characteristic ions and retention times of the target compounds are shown in table 1:
TABLE 1 characteristic ions and Retention times for the amino acids
Selection of characteristic ions of the amino acid derivative in the sample solution, different amino acid derivatives having various characteristic ions. The amino acid esterified derivative has a characteristic peak [ M-101 ]]+, where 101 represents the loss of molecular ion peak-COOC4H9. Alanine (Ala), valine (Val), proline (Pro) derivatives having a peak of [ M-101 ]]+. phenylalanine (Phe) and glutamic acid (Glu) have base peaks of 91 and 180, respectively threonine (Thr), serine (Ser), leucine (L eu), isoleucine (Ile) and aspartic acid (Asp) have base peaks of 57, 57, 69, 69 and 57, respectively, with a lower mass to charge ratio and more interference, thus selecting the second most intense characteristic ions 153, 139, 182, 182 and 240 as the detection ions.
S5, preparing amino acid mixed standard stock solutions, sequentially carrying out S3 operations on the amino acid mixed standard stock solutions with different solution mass concentrations to obtain sample stock solutions, carrying out GC-MS detection on the sample stock solutions respectively, detecting peak surfaces of characteristic ions of amino acid derivatives in the sample stock solutions, and carrying out a linear regression equation on the peak surfaces according to the solution mass concentrations to obtain a linear regression equation of the amino acids;
preparing amino acid mixed standard stock solution, namely weighing a certain amount of 10 amino acid solids respectively, preparing stock solution with the concentration of 1 g/L from 0.1 mol/L HCl to prepare stock solution with the concentration of 50m L to obtain 10 amino acid mixed standard solution, and performing linear regression analysis on the amino acid mixed standard stock solution by respectively taking the mixed standard solution with the concentrations of 0.1, 0.5, 1, 2, 5, 10, 20 and 30 mg/L, wherein the linear regression equation and the detection limit of each amino acid are obtained by taking the peak area of the characteristic ion of the corresponding amino acid derivative as an axis Y and the concentration as an axis X, and the following table 2:
TABLE 2 Standard Curve and correlation coefficient for each amino acid
As can be seen from the above table, the method shows good linear correlation, the correlation coefficient R2The detection limit of 10 amino acids is 2.3-13.9 mu g/L, wherein the detection limit is 0.992-0.999.
And S6, according to the amino acid linear regression equation in S5, calculating the content of the amino acid in the peak area and the peak emergence time of the characteristic ion of the amino acid derivative measured in S4.
The invention analyzes the free amino acid of the water sample collected by the sampling point, and selects 10 common amino acids in the water source as target objects, namely alanine, threonine, serine, valine, leucine, isoleucine, proline, aspartic acid, phenylalanine and glutamic acid. FIG. 1 is a chromatogram obtained by the amino acid detection method of this example for a standard substance.
The detection results of the CX and TH water plant raw water and the process section amino acid in the embodiment are as follows:
TABLE 3 FAAs content in raw water and process stage effluent from CX and TH waterworks
RW raw water, SEDI precipitation, SAF sand filtration, FW effluent, PREO pre-ozone, POSTO post-ozone, ACF active carbon unit μ g/L
Referring to FIGS. 2 to 3, the reliability of solid phase extraction and derivatization was verified by the spiking recovery test, 10 amino acid solutions of 1L concentrations of 5, 10 and 20. mu.g/L were prepared with pure water, tap water and raw water, respectively, enriched by solid phase extraction, and the extract was derivatized and injected into GC-MS for quantitative analysis, and the recovery of various free amino acids is shown in Table 4.
TABLE 4 recovery of amino acids in pure, tap and raw water with spiking
As can be seen from the above table, the total recovery rate of 10 amino acids is about 80%, and similar recovery rates are achieved under three different water quality conditions and 3 different standard adding concentrations (5, 10 and 20 μ g/L). The recovery rates of Ala, Val, L eu, Ile, Pro and Phe in the three water sample standard adding methods are all greater than 80%.
In conclusion, the invention effectively realizes the enrichment and purification of the amino acid by adopting the specific solid phase extraction-derivatization pretreatment and the gas chromatography-mass spectrometer for detecting the trace amino acid in the water source, avoids the interference of other impurities, and has low detection limit and good linearity. Makes up the defects of the existing method for detecting trace amino acid in water sources, and the method is easier to be applied to the detection of more amino acid contents.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (10)
1. A solid phase extraction-gas chromatography-mass spectrometry method for simultaneously detecting various trace free amino acids in a water source is characterized by comprising the following steps:
s1, collecting a water sample;
s2, purifying and enriching the water sample in the S1, and obtaining the purified and enriched water sample by adopting a solid phase extraction mode;
s3, performing esterification derivatization treatment on the water sample treated in the S2 to obtain a sample solution;
s4, detecting the sample solution obtained in the S3 by adopting GC-MS, and measuring the peak area and the peak emergence time of the characteristic ions of the amino acid derivatives in the sample solution;
s5, preparing amino acid mixed standard stock solutions, sequentially carrying out S3 operations on the amino acid mixed standard stock solutions with different solution mass concentrations to obtain sample stock solutions, carrying out GC-MS detection on the sample stock solutions respectively, detecting peak surfaces of characteristic ions of amino acid derivatives in the sample stock solutions, and carrying out a linear regression equation on the peak surfaces according to the solution mass concentrations to obtain a linear regression equation of the amino acids;
and S6, according to the amino acid linear regression equation in S5, calculating the content of the amino acid in the peak area and the peak emergence time of the characteristic ion of the amino acid derivative measured in S4.
2. The method of claim 1, wherein the step of performing solid phase extraction in S2 comprises the steps of,
step 1, adjusting the pH value of a water sample to 1.3 by using hydrochloric acid before loading the water sample on a column, and rinsing the activated column by using 4.5m L methanol and 9m L hydrochloric acid;
step 2, passing the water sample through the column at the speed of 2m L/min, and then eluting by taking 9m L methanol solution containing 5% ammonia water for three times, wherein 3m L is used for elution each time to obtain eluent;
and 3, drying the eluent by using a nitrogen blowing instrument, and dissolving the eluent by using hydrochloric acid with the concentration of 1m L to finally obtain a purified and enriched water sample.
3. The method of claim 2, wherein the hydrochloric acid is present at a concentration of 0.1 mol/L.
4. The method for simultaneously detecting multiple trace free amino acids in a water source by solid phase extraction-gas chromatography-mass spectrometry as claimed in claim 1, wherein the esterification and derivatization treatment in S3 comprises the following steps;
step 1, taking 100 mu L of water sample purified and enriched in S2 to a reaction tube, adding 50 mu L of dichloromethane, blowing the water sample to a nitrogen blowing instrument for drying, adding 50 mu L of hydrochloric acid-n-butanol, and putting the mixture into a 120 ℃ oven for esterification for 60min to obtain a sample A;
step 2, adding 50 mu L dichloromethane, 100 mu L ethyl acetate and 100 mu L trifluoroacetic anhydride into the sample A, and sealing the tube to obtain a sample B;
and step 3: placing the reaction tube provided with the sample B into an oven for acylation at 120 ℃ for 30 min;
and 4, blowing the acylated sample B by using a nitrogen blowing instrument, and adding 500 mu L of dichloromethane for dissolution to obtain a sample solution.
5. The method of claim 4, wherein the concentration of the hydrochloric acid-n-butanol is 3.5 mol/L.
6. The solid-phase extraction-gas chromatography-mass spectrometry method for simultaneously detecting multiple trace free amino acids in a water source is characterized in that the GC-MS detection comprises the following conditions that the temperature of a vaporization chamber is 280 ℃, carrier gas is high-purity He, the flow rate is 1.0m L/min, the ionization energy of an EI source is 70ev, the temperature is 200 ℃, the filament current is 220mA, the interface temperature is 250 ℃, the temperature of a chromatographic column is 70-300 ℃, the retention time is 2-15 min, the temperature rise speed is 15 ℃/min, the qualitative scanning range of mass is 40-600amu by using a full scanning mode, the quantitative scanning range of mass is 40-600amu by using an SIM mode, and the ion scanning m/z is selected from alanine 140, threonine 153, serine 139, valine 168, leucine 182, isoleucine 182, proline 166, aspartic acid 240, phenylalanine 91 and glutamic acid 180.
7. The solid-phase extraction-gas chromatography-mass spectrometry combination method for simultaneously detecting multiple trace free amino acids in a water source as claimed in claim 1, wherein the amino acid mixed standard stock solution in S5 is formed by mixing different kinds of amino acid stock solutions, and the preparation of the amino acid stock solution comprises the following steps of weighing amino acid solids and preparing 50m L stock solution by using 0.1 mol/L HCl.
8. The method of claim 7, wherein the amino acid solids comprise alanine, threonine, serine, valine, leucine, isoleucine, proline, aspartic acid, phenylalanine, and glutamic acid.
9. The method of claim 1, wherein the amino acid mixed standard stock solution has a solution mass concentration of 0.1, 0.5, 1, 2, 5, 10, 20, and 30 mg/L.
10. The method of claim 1, wherein the linear regression analysis in S5 is performed by using the peak area of the characteristic ion of the amino acid derivative as the Y axis and the concentration as the X axis.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106645486A (en) * | 2016-12-28 | 2017-05-10 | 南京大学 | Method for measuring residual quantity of glyphosate in soil employing liquid chromatography-high-resolution mass spectrometer |
| CN110018266A (en) * | 2019-02-15 | 2019-07-16 | 广州市妇女儿童医疗中心 | A kind of method of 48 kinds of amino acid of fast quantitative analysis |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106645486A (en) * | 2016-12-28 | 2017-05-10 | 南京大学 | Method for measuring residual quantity of glyphosate in soil employing liquid chromatography-high-resolution mass spectrometer |
| CN110018266A (en) * | 2019-02-15 | 2019-07-16 | 广州市妇女儿童医疗中心 | A kind of method of 48 kinds of amino acid of fast quantitative analysis |
Non-Patent Citations (5)
| Title |
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| YANG YULONG ET AL.: "Occurrence of free amino acids in the source waters of Zhejiang Province, China, and their removal and transformation in drinking water systems", 《WATER》 * |
| 倪梦婷: "水环境中氨基酸—含氮消毒副产物生成研究", 《中国优秀硕士学位论文全文数据库 工程科技II辑》 * |
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Application publication date: 20200710 |