CN112014485A - Method for measuring geosmin and 2-methylisoborneol in sediment - Google Patents
Method for measuring geosmin and 2-methylisoborneol in sediment Download PDFInfo
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- CN112014485A CN112014485A CN201910462731.0A CN201910462731A CN112014485A CN 112014485 A CN112014485 A CN 112014485A CN 201910462731 A CN201910462731 A CN 201910462731A CN 112014485 A CN112014485 A CN 112014485A
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- temperature
- methylisoborneol
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- sediment
- geosmin
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- LFYXNXGVLGKVCJ-FBIMIBRVSA-N 2-methylisoborneol Chemical compound C1C[C@@]2(C)[C@](C)(O)C[C@@H]1C2(C)C LFYXNXGVLGKVCJ-FBIMIBRVSA-N 0.000 title claims abstract description 26
- LFYXNXGVLGKVCJ-UHFFFAOYSA-N 2-methylisoborneol Natural products C1CC2(C)C(C)(O)CC1C2(C)C LFYXNXGVLGKVCJ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- DTGKSKDOIYIVQL-UHFFFAOYSA-N dl-isoborneol Natural products C1CC2(C)C(O)CC1C2(C)C DTGKSKDOIYIVQL-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000013049 sediment Substances 0.000 title claims abstract description 26
- JLPUXFOGCDVKGO-TUAOUCFPSA-N (-)-geosmin Chemical compound C1CCC[C@]2(O)[C@@H](C)CCC[C@]21C JLPUXFOGCDVKGO-TUAOUCFPSA-N 0.000 title claims abstract description 17
- 239000001075 (4R,4aR,8aS)-4,8a-dimethyl-1,2,3,4,5,6,7,8-octahydronaphthalen-4a-ol Substances 0.000 title claims abstract description 17
- JLPUXFOGCDVKGO-UHFFFAOYSA-N dl-geosmin Natural products C1CCCC2(O)C(C)CCCC21C JLPUXFOGCDVKGO-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229930001467 geosmin Natural products 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000000605 extraction Methods 0.000 claims abstract description 28
- 238000001319 headspace solid-phase micro-extraction Methods 0.000 claims abstract description 12
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims abstract description 7
- 238000005070 sampling Methods 0.000 claims abstract description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 8
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 8
- 230000005540 biological transmission Effects 0.000 claims description 4
- 238000004587 chromatography analysis Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 238000004451 qualitative analysis Methods 0.000 claims description 4
- 238000004445 quantitative analysis Methods 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 230000003595 spectral effect Effects 0.000 claims description 3
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 2
- 241000233866 Fungi Species 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- -1 polydimethylsiloxane Polymers 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- KZAOEMMZRGEBST-UHFFFAOYSA-N Odorine Natural products CCC(C)C(=O)NC1CCCN1C(=O)C=CC1=CC=CC=C1 KZAOEMMZRGEBST-UHFFFAOYSA-N 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 238000004401 flow injection analysis Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229930000044 secondary metabolite Natural products 0.000 description 1
- 238000002470 solid-phase micro-extraction Methods 0.000 description 1
- 238000012421 spiking Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
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Classifications
-
- 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
-
- 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
-
- 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
Abstract
The method aims at overcoming the defects of the existing sample detection technology, and particularly relates to a method for determining geosmin and 2-methylisoborneol in sediments, which comprises the following steps: sampling, headspace solid phase microextraction and GC-MS analysis; according to the invention, by comparing the extraction effects of different types of extraction heads, the extraction conditions such as extraction time and temperature are optimized, and a new method for simultaneously determining geosmin and 2-methylisoborneol in the sediment by headspace solid-phase microextraction/gas chromatography/mass spectrometry is established.
Description
Technical Field
The invention relates to a method for measuring chemical substances, in particular to a method for measuring geosmin and 2-methylisoborneol in sediments.
Background
The geosmin and the 2-methylisoborneol are secondary metabolites which are continuously secreted and released by algae and fungi and have peculiar smell, and are one of main substances causing the earthy and musty smell of the water body, the algae and the fungi are deposited at the bottom of the water body after death and form sediments with mud, the sediments also contain the odorous substances, and the odorous substances in the sediments are released into the water body again under the mutation of external conditions (such as water flow and strong wind), so that the odorous substances in the water body are increased; at present, a plurality of methods for measuring 2-methylisoborneol in water exist, and the measurement of 2-methylisoborneol in sediments is not reported, so that a method for measuring 2-methylisoborneol in sediments is necessary to be established.
Disclosure of Invention
In order to solve the problems, the invention provides a method for measuring geosmin and 2-methylisoborneol in sediments.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for measuring geosmin and 2-methylisoborneol in sediments is characterized in that: comprises the following steps;
a: sampling, taking a part of about 2g of sediment into a 20ml headspace sample bottle, adding 2.0g of sodium chloride, screwing a bottle cap, and detecting. Another part (about 2 g) is used for measuring the water content of the sample;
b: performing headspace solid phase microextraction, and selecting a DVB/CAR/PDMS extraction head with the diameter of 50/30 mu m; extraction conditions are as follows: the heating temperature is 70 ℃; the extraction time is 35 min; the depth of the extraction head inserted into the bottle is 25 mm; the resolving time is 5 min; the rotation speed of the heater is 500 rpm;
c: and (3) performing GC-MS analysis, namely after the headspace solid phase microextraction is finished, inserting an extraction head into a gas sample inlet to analyze for 5min at 250 ℃, and realizing the qualitative and quantitative analysis of the 2-methylisoborneol in the sediment.
Further, chromatographic conditions: DB-624 capillary chromatography column (30 m 0.25 mm 1.4 μm, Agilent Corp.); high purity helium (99.999%) at a flow rate of 1.0 mL/min; column temperature: the initial temperature is kept at 40 ℃ for 2 min, the temperature is increased to 220 ℃ at the speed of 10 ℃/min, and the temperature is kept for 10 min; sample inlet temperature: injecting samples at 250 ℃ without shunting; spectral conditions: EI source electron energy is 70 eV; ion source temperature: 230 ℃; temperature of the quadrupole rods: 150 ℃; transmission line temperature: 250 ℃; the collection mode is as follows: full SCAN (SCAN) qualitative, ion (SIM) mode selected quantitative; solvent retardation: and 5 min.
Drawing a standard curve: quantifying by adopting an external standard method; mixing 100mg/L geosmin and 2-methylisoborneol to obtain a standard solution, diluting 1000 times with methanol to obtain a standard use solution of 100 μ g/L, and storing in refrigerator for cold storage; 2.00g of quartz sand, 10.0ml of saturated sodium chloride solution and a certain amount of standard use solution are sequentially added into 5 overhead bottles, sealing is immediately carried out, and calibration curves of 6-point different concentration series with target compounds of 0.04ng, 0.10ng, 0.20ng, 0.50ng, 1.00ng and 2.00ng are prepared. Oscillating the prepared standard series samples on an oscillator for 10min at the frequency of 150 times/min, performing headspace solid phase microextraction according to the step B, and then analyzing according to the step C; and drawing a standard curve by taking the peak area of the characteristic ion peak of the 2-methylisoborneol as the abscissa and the mass as the ordinate.
Sediment sample results calculation:
in the formula:
ng/kg of olfactory substance content in the sample;
m1sample size (wet weight), g;
omega-dry matter content of the sample,%.
The invention has the beneficial effects that: according to the invention, by comparing the extraction effects of different types of extraction heads, the extraction conditions such as extraction time and temperature are optimized, and a new method for simultaneously determining geosmin and 2-methylisoborneol in the sediment by headspace solid-phase microextraction/gas chromatography/mass spectrometry is established.
Drawings
FIG. 1 is a graph of linear range, correlation coefficient, and detection limit for a method according to an embodiment of the invention;
FIG. 2 is a graph of recovery rate (n-7) and precision for an odorin and 2-methylisoborneol spiking test according to an embodiment of the present invention;
FIG. 3 is a chromatogram of 20ng/kg geosmin and 2-methylisoborneol according to an embodiment of the present invention.
Detailed Description
In order to make the technical solution of the present invention more apparent, the present invention is further described with reference to the following embodiments.
As shown in fig. 1 to 3, a method for measuring geosmin and 2-methylisoborneol in sediment according to an embodiment of the present invention is characterized in that: comprises the following steps;
a: sampling, taking a part of about 2g of sediment into a 20ml headspace sample bottle, adding 2.0g of sodium chloride, screwing a bottle cap, and detecting. Another part (about 2 g) is used for measuring the water content of the sample;
b: performing headspace solid phase microextraction, and selecting a DVB/CAR/PDMS extraction head with the diameter of 50/30 mu m; extraction conditions are as follows: the heating temperature is 70 ℃; the extraction time is 35 min; the depth of the extraction head inserted into the bottle is 25 mm; the resolving time is 5 min; the rotation speed of the heater is 500 rpm;
c: and (3) performing GC-MS analysis, namely after the headspace solid phase microextraction is finished, inserting an extraction head into a gas sample inlet to analyze for 5min at 250 ℃, and realizing the qualitative and quantitative analysis of the 2-methylisoborneol in the sediment.
Further, chromatographic conditions: DB-624 capillary chromatography column (30 m 0.25 mm 1.4 μm, Agilent Corp.); high purity helium (99.999%) at a flow rate of 1.0 mL/min; column temperature: the initial temperature is kept at 40 ℃ for 2 min, the temperature is increased to 220 ℃ at the speed of 10 ℃/min, and the temperature is kept for 10 min; sample inlet temperature: injecting samples at 250 ℃ without shunting; spectral conditions: EI source electron energy is 70 eV; ion source temperature: 230 ℃; temperature of the quadrupole rods: 150 ℃; transmission line temperature: 250 ℃; the collection mode is as follows: full SCAN (SCAN) qualitative, ion (SIM) mode selected quantitative; solvent retardation: and 5 min.
As shown in fig. 1-3, the raw materials and equipment used in the examples of the present invention are as follows:
agilent 7890B-5977C gas chromatography/mass spectrometer; gerstel MPS2 model multifunctional autosampler (containing solid phase microextraction); supelco 50/30 μm polydimethylsiloxane/activated carbon/divinylbenzene (DVB/CAR/PDMS), 100 μm Polydimethylsiloxane (PDMS).
The mixed standard concentration of geosmin and 2-methylisoborneol in methanol is 100mg/L (Sigma company), the methanol is chromatographic pure (Tedia reagent company in the United states), and the hydrochloric acid and sodium chloride are analytical pure (chemical reagent company in national drug group).
In this example, the sediment at 3 rd lake area of suzhou city, Jiangsu province was analyzed by the following specific method:
a: and (6) sampling. Collecting a proper amount of sample to the bottom of the sample bottle, quickly removing the sample at the thread part of the sample bottle (the sample is difficult to be adhered to the bottle mouth in lake sampling), and sealing the sample bottle. All samples were taken in parallel at least 2 parts (about 2.0g per sample) and 1 part was taken for the determination of the water content of the samples. Before measurement, the weight was measured again and 10.0ml of saturated saline was added.
B: and (4) headspace solid phase microextraction. Selecting a DVB/CAR/PDMS extraction head with the diameter of 50/30 mu m; extraction conditions are as follows: the heating temperature is 70 ℃; the extraction time is 35 min; the depth of the extraction head inserted into the bottle is 25 mm; the resolving time is 5 min; the heater speed was 500 rpm.
C: and (5) performing GC-MS analysis. After the headspace solid phase microextraction is finished, the extraction head is inserted into a gas sample inlet to be analyzed for 5min at the temperature of 250 ℃, so that the qualitative and quantitative analysis of the 2-methylisoborneol in the sediment is realized. Wherein: chromatographic conditions are as follows: DB-624 capillary chromatography column (30 m 0.25 mm 1.4 μm, Agilent Corp.); high purity helium (99.999%) at a flow rate of 1.0 mL/min; column temperature: the initial temperature is kept at 40 ℃ for 2 min, the temperature is increased to 220 ℃ at the speed of 10 ℃/min, and the temperature is kept for 10 min; sample inlet temperature: no split-flow injection was carried out at 250 ℃.
Mass spectrum conditions: EI source electron energy is 70 eV; ion source temperature: 230 ℃; temperature of the quadrupole rods: 150 ℃; transmission line temperature: 250 ℃; the collection mode is as follows: full SCAN (SCAN) qualitative, ion (SIM) mode selected quantitative; solvent retardation: and 5 min.
Determination of actual sample geosmin and 2-methylisoborneol
| Sample name | Geosmin/(ng kg-1) | 2-methylisoborneol (ng.kg-1) |
| Sample 1 | <4 | 5 |
| Sample 2 | 6 | 7 |
| Sample 3 | 10 | 13 |
The above embodiments may be combined with each other and further implemented without being mutually opposed.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (2)
1. A method for measuring geosmin and 2-methylisoborneol in sediments is characterized in that: comprises the following steps;
a: sampling, namely taking about 2g of sediment into a 20ml headspace sample bottle, adding 2.0g of sodium chloride, screwing a bottle cap, and measuring the water content of the sample, wherein about 2g of sediment is taken;
b: performing headspace solid phase microextraction, and selecting a DVB/CAR/PDMS extraction head with the diameter of 50/30 mu m; extraction conditions are as follows: the heating temperature is 70 ℃; the extraction time is 35 min; the depth of the extraction head inserted into the bottle is 25 mm; the resolving time is 5 min; the rotation speed of the heater is 500 rpm;
c: and (3) performing GC-MS analysis, namely after the headspace solid phase microextraction is finished, inserting an extraction head into a gas sample inlet to analyze for 5min at 250 ℃, and realizing the qualitative and quantitative analysis of the 2-methylisoborneol in the sediment.
2. The method of claim 1 for determining geosmin and 2-methylisoborneol in sediments, comprising the steps of: chromatographic conditions are as follows: DB-624 capillary chromatography column (30 m 0.25 mm 1.4 μm, Agilent Corp.); high purity helium (99.999%) at a flow rate of 1.0 mL/min; column temperature: the initial temperature is kept at 40 ℃ for 2 min, the temperature is increased to 220 ℃ at the speed of 10 ℃/min, and the temperature is kept for 10 min; sample inlet temperature: injecting samples at 250 ℃ without shunting; spectral conditions: EI source electron energy is 70 eV; ion source temperature: 230 ℃; temperature of the quadrupole rods: 150 ℃; transmission line temperature: 250 ℃; the collection mode is as follows: full SCAN (SCAN) qualitative, ion (SIM) mode selected quantitative; solvent retardation: and 5 min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112730650A (en) * | 2020-12-15 | 2021-04-30 | 湖南微谱检测技术有限公司 | Method for enriching ultra-trace organic matters in large-volume water |
| CN113176355A (en) * | 2021-04-25 | 2021-07-27 | 中国水产科学研究院淡水渔业研究中心 | Pretreatment method for detecting soil odor substances in aquatic products |
| CN113176356A (en) * | 2021-04-25 | 2021-07-27 | 中国水产科学研究院淡水渔业研究中心 | Pretreatment method for detecting soil odor substances in aquaculture water |
| CN113960236A (en) * | 2021-10-11 | 2022-01-21 | 大连海洋大学 | Method for determining geosmin and dimethyl isoborneol in fish body based on rapid pretreatment technology |
-
2019
- 2019-05-30 CN CN201910462731.0A patent/CN112014485A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 黎莉 等: "HS-SPME-GC-MS法测定水中2-甲基异冰片及土臭素" * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112730650A (en) * | 2020-12-15 | 2021-04-30 | 湖南微谱检测技术有限公司 | Method for enriching ultra-trace organic matters in large-volume water |
| CN112730650B (en) * | 2020-12-15 | 2022-08-09 | 湖北微谱技术有限公司 | Method for enriching ultra-trace organic matters in large-volume water |
| CN113176355A (en) * | 2021-04-25 | 2021-07-27 | 中国水产科学研究院淡水渔业研究中心 | Pretreatment method for detecting soil odor substances in aquatic products |
| CN113176356A (en) * | 2021-04-25 | 2021-07-27 | 中国水产科学研究院淡水渔业研究中心 | Pretreatment method for detecting soil odor substances in aquaculture water |
| CN113176355B (en) * | 2021-04-25 | 2022-08-09 | 中国水产科学研究院淡水渔业研究中心 | Pretreatment method for detecting soil odor substances in aquatic products |
| CN113960236A (en) * | 2021-10-11 | 2022-01-21 | 大连海洋大学 | Method for determining geosmin and dimethyl isoborneol in fish body based on rapid pretreatment technology |
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