CN113075321A - Detection and analysis method for thioether odor substances in drinking water - Google Patents
Detection and analysis method for thioether odor substances in drinking water Download PDFInfo
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- CN113075321A CN113075321A CN202110328804.4A CN202110328804A CN113075321A CN 113075321 A CN113075321 A CN 113075321A CN 202110328804 A CN202110328804 A CN 202110328804A CN 113075321 A CN113075321 A CN 113075321A
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- 239000000126 substance Substances 0.000 title claims abstract description 33
- 239000003651 drinking water Substances 0.000 title claims abstract description 28
- 235000020188 drinking water Nutrition 0.000 title claims abstract description 28
- 150000003568 thioethers Chemical class 0.000 title claims abstract description 27
- 238000001514 detection method Methods 0.000 title claims abstract description 20
- 238000004458 analytical method Methods 0.000 title claims abstract description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 claims description 22
- YWHLKYXPLRWGSE-UHFFFAOYSA-N Dimethyl trisulfide Chemical compound CSSSC YWHLKYXPLRWGSE-UHFFFAOYSA-N 0.000 claims description 20
- 239000003480 eluent Substances 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000004252 FT/ICR mass spectrometry Methods 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract 1
- 238000011160 research Methods 0.000 description 13
- CETBSQOFQKLHHZ-UHFFFAOYSA-N Diethyl disulfide Chemical compound CCSSCC CETBSQOFQKLHHZ-UHFFFAOYSA-N 0.000 description 5
- 239000012286 potassium permanganate Substances 0.000 description 5
- VLXBWPOEOIIREY-UHFFFAOYSA-N dimethyl diselenide Natural products C[Se][Se]C VLXBWPOEOIIREY-UHFFFAOYSA-N 0.000 description 4
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 description 3
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000013558 reference substance Substances 0.000 description 3
- JOZDADPMWLVEJK-UHFFFAOYSA-N 1-pentylsulfanylpentane Chemical compound CCCCCSCCCCC JOZDADPMWLVEJK-UHFFFAOYSA-N 0.000 description 2
- 239000004155 Chlorine dioxide Substances 0.000 description 2
- ZERULLAPCVRMCO-UHFFFAOYSA-N Dipropyl sulfide Chemical compound CCCSCCC ZERULLAPCVRMCO-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 235000019398 chlorine dioxide Nutrition 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 230000000813 microbial effect Effects 0.000 description 2
- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 241000272814 Anser sp. Species 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000544061 Cuculus canorus Species 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000001640 nerve ending Anatomy 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000009287 sand filtration Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- General Health & Medical Sciences (AREA)
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Abstract
The invention relates to a detection and analysis method for thioether odor substances in drinking water. The detection analysis method adopts a GC-MS method, and comprises the following steps: accurately preparing a certain amount of drinking water to be detected; eluting by adopting a mobile phase, wherein the mobile phase is a mixed solution of acetonitrile and water, and the adopted mobile phase is the acetonitrile and the water in a volume ratio of 40-60: 50-70. The method has high detection sensitivity and accurate detection result.
Description
Technical Field
The invention relates to the technical field of detection and extraction of thioether substances, in particular to a detection and analysis method of thioether odor substances in drinking water.
Background
The odor problem of drinking water (Taste and Ordor, T & O) is one of the important factors affecting the water quality of drinking water sources in recent years, which is ubiquitous in the world and has a growing trend, the odor substance can cause the odor of water bodies, part of the odor substance can harm the health of human bodies, the research on the odor problem of water bodies is started in the middle of 20 th century abroad, the odor problem of drinking water becomes more and more serious, the odor problem becomes one of the research hot spots of water environment in the world, the research on the odor problem of drinking water in China is relatively late, the related experiments and research are just started, the thioether odor substance is a sulfur-containing organic substance which has serious influence and is released by the growth and death metabolism of algae, the thioether odor substance has higher odor activity intensity and concentration level in the actual water body, Dimethyl disulfide (DMDS ), Diethyl disulfide (Diethyl disulfide, DEDS), amyl thioether (DAS) and propyl thioether (DPS) are some sulfides causing serious problems in thioether smelly substances, and research shows that the removal effect of traditional methods such as coagulation, precipitation, sand filtration and the like on the smelly substances is very slight, but the thioether substances are easy to remove through oxidation, and research on removing methyl sulfide and dimethyl trithioether by potassium permanganate is carried out in the related field at present, and the result shows that the potassium permanganate has a good removal effect on the methyl sulfide and the dimethyl trithioether, but a certain time (2h) is needed for complete removal, and the reaction of the potassium permanganate with the methyl sulfide and the dimethyl trithioether conforms to a secondary kinetic reaction process. Although the above research shows that potassium permanganate has good removal effect on part of smelly substances; the research of removing dimethyl trisulfide in water body by potassium ferrate is carried out by cuckoo goose, Zhang Yang Hua and the like, and 92.5 percent of dimethyl trisulfide is removed in the time that the potassium ferrate is oxidized for 1 min; regarding the research on thioether substances, similar to the research on oxidizing DMDS by chlorine dioxide, the research on removing DMDS by methods such as microbial filtration, microbial removal, photocatalysis, etc. is also conducted, but the research does not relate to thioether smelly substances such as DAS, and the research on removing DMDS by chlorine dioxide in the field of drinking water is few and has a single oxidation mode.
At present, the thioether odor substances are removed mainly by adopting an oxidation mode, and oxidizing agents often bring various problems, for example, potassium permanganate easily produces heavy metal pollution, so that the thioether substances in a water body must be quantitatively detected and analyzed.
Dimethyl disulfide and dimethyl trisulfide are two sulfur-containing compounds with special odor, are often present in polluted water bodies, have low odor threshold values and strong odor and can damage human nerve endings.
Disclosure of Invention
The invention aims to provide a method for detecting and analyzing thioether odor substances in drinking water.
The invention adopts the following technical scheme that:
a detection and analysis method for thioether odor substances in drinking water adopts a GC-MS method, and comprises the following steps:
(1) accurately preparing a certain amount of drinking water to be detected;
(2) and eluting by adopting a mobile phase, wherein the mobile phase is a mixed solution of acetonitrile and water.
Preferably, the amount of drinking water accurately prepared is 5-20 ml.
Wherein in the mobile phase, the volume ratio of acetonitrile to water is 40-60: 50-70.
Preferably, elution is carried out with an eluent having a volume ratio of acetonitrile to water of 50:50 in 0-5 minutes.
Preferably, elution is carried out with an eluent having a volume ratio of acetonitrile to water of 45:55 at 5-10 minutes.
Wherein, at 0-5 min, the eluting substance is dimethyl disulfide, and the retention time is 1.563 min.
Wherein, the elution substance is dimethyl trisulfide with the retention time of 8.146min at 5-10 min.
Preferably, the conditions of the GC-MS are as follows: an Agilent1100 high performance liquid chromatograph is provided with a quaternary pump solvent elution system, an automatic sample injector and an ultraviolet detector; the column was a YMC-Pack-ODS-AC18 column (250 mm. times.4.6 mm. i.d.,5 μm), column temperature: 30 ℃ at 10 ℃/min up to 220 ℃, flow rate: 1.0mL/min, and the injection port temperature is 230 ℃; high resolution mass spectrometer: brukeraapex IVFT-MS.
Preferably, the length of the chromatographic column is 250mm, the diameter is 4.6mm, and the particle size of the packing is 5 μm; the detection wavelength of the detector is 218-222 nm.
Wherein the detection limit of dimethyl disulfide<0.0030ng·mL-1(ii) a Detection limit of dimethyl trisulfide<0.0015ng·mL-1。
Drawings
FIG. 1 is a liquid chromatogram of the thioether odorant of the present invention.
Examples
The invention is further illustrated by the following examples. It should be understood that the method described in the examples is only for illustrating the present invention and not for limiting the present invention, and that simple modifications of the preparation method of the present invention based on the concept of the present invention are within the scope of the claimed invention. All starting materials and solvents used in the examples are commercially available products of the corresponding purity.
The content of the modified substances in the drinking water was determined by GC-MS. The detection conditions are as follows: the GC-MS conditions were: an Agilent1100 high performance liquid chromatograph is provided with a quaternary pump solvent elution system, an automatic sample injector and an ultraviolet detector; the column was a YMC-Pack-ODS-AC18 column (250 mm. times.4.6 mm. i.d.,5 μm), column temperature: 30 ℃ at 10 ℃/min up to 220 ℃, flow rate: 1.0mL/min, and the injection port temperature is 230 ℃; high resolution mass spectrometer: brukeraapex IV FT-MS. The length of the chromatographic column is 250mm, the diameter is 4.6mm, and the particle size of the filler is 5 μm; the detection wavelength of the detector is 218-222 nm.
Accurately weighing 10mL of dimethyl disulfide and a dimethyl trisulfide reference substance (Sigma) to dissolve by using acetonitrile and water, dissolving in 20mL of acetonitrile and water, shaking, finally preparing the concentration of the reference substance to be 25, 50, 100, 200, 400 and 500 mu g/mL, passing through a 0.45 mu m organic filter membrane, taking the logarithm of the peak area as the ordinate, taking the logarithm of the concentration of the reference substance as the abscissa, drawing a standard curve and carrying out regression calculation, wherein the regression equation is that Y is 1.4377X +3.5492, and r is 0.9996. Then 10mL of drinking water (three batches) is weighed, shaken up, filtered through a 0.45 mu m organic filter membrane with the sample amount of 20 mu L, and eluted by adopting eluent with the volume ratio of acetonitrile to water of 50:50 in 0-5 minutes. And eluting with an eluent with the volume ratio of acetonitrile to water being 45:55 in 5-10 minutes. At 0-5 min, the eluting material was dimethyldisulfide, with a retention time of 1.563 min. At 5-10 min, the eluted material was dimethyl trisulfide, and the retention time was 8.146 min. The measured contents and detection limits are shown in the following table by calculation according to the linear regression equation and standard sample data:
| components | Detection Limit (ng. mL)-1) | Content (μ g. L)-1) |
| Dimethyl disulfide | 0.0026 | 0.38 |
| Dimethyl trisulfide | 0.0012 | 0.42 |
Claims (10)
1. A detection and analysis method for thioether odor substances in drinking water adopts a GC-MS method, and is characterized by comprising the following steps:
(1) accurately preparing a certain amount of drinking water to be detected;
(2) and eluting by adopting a mobile phase, wherein the mobile phase is a mixed solution of acetonitrile and water.
2. The method for detecting and analyzing thioether odor substances in drinking water according to claim 1, wherein the method comprises the following steps: the amount of the drinking water accurately prepared is 5 to 20 milliliters.
3. The method for detecting and analyzing thioether odor substances in drinking water according to claim 1, wherein the method comprises the following steps: in the mobile phase, the volume ratio of acetonitrile to water is 40-60: 50-70.
4. The method for detecting and analyzing thioether odor substances in drinking water according to claim 1, wherein the method comprises the following steps: and eluting with an eluent with a volume ratio of acetonitrile to water of 50:50 at 0-5 minutes.
5. The method for detecting and analyzing thioether odor substances in drinking water according to claim 1, wherein the method comprises the following steps: and eluting with an eluent with the volume ratio of acetonitrile to water being 45:55 in 5-10 minutes.
6. The method for detecting and analyzing thioether odor substances in drinking water according to claim 4, wherein the method comprises the following steps: at 0-5 min, the eluting material was dimethyldisulfide, with a retention time of 1.563 min.
7. The method for detecting and analyzing thioether odor substances in drinking water according to claim 5, wherein: at 5-10 min, the eluted material was dimethyl trisulfide, and the retention time was 8.146 min.
8. The method for detecting and analyzing thioether odor substances in drinking water according to claim 1, wherein the GC-MS conditions are as follows: an Agilent1100 high performance liquid chromatograph is provided with a quaternary pump solvent elution system, an automatic sample injector and an ultraviolet detector; the column was a YMC-Pack-ODS-AC18 column (250 mm. times.4.6 mm. i.d.,5 μm), column temperature: 30 ℃ at 10 ℃/min up to 220 ℃, flow rate: 1.0mL/min, and the injection port temperature is 230 ℃; high resolution mass spectrometer: brukeraapex IV FT-MS.
9. The method for detecting and analyzing thioether odor substances in drinking water according to claim 8, wherein the method comprises the steps of: the length of the chromatographic column is 250mm, the diameter is 4.6mm, and the particle size of the filler is 5 μm; the detection wavelength of the detector is 218-222 nm.
10. The method for detecting and analyzing thioether odor substances in drinking water according to claim 8, wherein the method comprises the steps of: detection limit of dimethyl disulfide<0.0030ng·mL-1(ii) a Detection limit of dimethyl trisulfide<0.0015ng·mL-1。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114674964A (en) * | 2022-05-26 | 2022-06-28 | 北京建筑大学 | Method for simultaneously measuring various thioether smelly substances in drinking water |
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| US20140311217A1 (en) * | 2013-04-23 | 2014-10-23 | Hyundai Motor Company | Method for detecting fishy water odor from air conditioner, reproducing fishy water odor and preparing corresponding fishy water odor composition |
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| CN105388224A (en) * | 2015-10-17 | 2016-03-09 | 舟山市食品药品检验检测研究院 | Method for detecting 6 types of sulfur-containing smelly substances in aquatic product |
| CN111474274A (en) * | 2020-04-28 | 2020-07-31 | 上海大学 | Method for simultaneously measuring various thioether smelly substances in water body |
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- 2021-03-27 CN CN202110328804.4A patent/CN113075321A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140311217A1 (en) * | 2013-04-23 | 2014-10-23 | Hyundai Motor Company | Method for detecting fishy water odor from air conditioner, reproducing fishy water odor and preparing corresponding fishy water odor composition |
| CN105067737A (en) * | 2015-07-24 | 2015-11-18 | 同济大学 | Detection method for odor substances in water environment |
| CN105388224A (en) * | 2015-10-17 | 2016-03-09 | 舟山市食品药品检验检测研究院 | Method for detecting 6 types of sulfur-containing smelly substances in aquatic product |
| CN111474274A (en) * | 2020-04-28 | 2020-07-31 | 上海大学 | Method for simultaneously measuring various thioether smelly substances in water body |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114674964A (en) * | 2022-05-26 | 2022-06-28 | 北京建筑大学 | Method for simultaneously measuring various thioether smelly substances in drinking water |
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