CN106248827B - Extraction and detection method of 2, 4-decadienal - Google Patents
Extraction and detection method of 2, 4-decadienal Download PDFInfo
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- CN106248827B CN106248827B CN201610625089.XA CN201610625089A CN106248827B CN 106248827 B CN106248827 B CN 106248827B CN 201610625089 A CN201610625089 A CN 201610625089A CN 106248827 B CN106248827 B CN 106248827B
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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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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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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
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- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
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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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- 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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- G01N2030/146—Preparation by elimination of some components using membranes
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Abstract
The invention relates to an extraction and detection method of 2, 4-decadienal, which comprises the following steps: accurately weighing 0.2g of powder microcapsule containing 2, 4-decadienal, placing the powder microcapsule into a 10mL centrifuge tube, sucking 2mL of water by using a 1mL pipette to dissolve the powder microcapsule, adding 4mL of organic solvent after dissolving, carrying out ultrasonic treatment for 1min, standing for 2min to stratify, sucking 1mL of supernatant, adding 0.2g of anhydrous sodium sulfate, standing for 12h, and then passing through a membrane (0.22um organic filter membrane), thus obtaining the liquid to be detected. The method is simple and has small error.
Description
Technical Field
The invention relates to a detection method, in particular to a method for measuring 2, 4-decadienal.
Background
2, 4-decadienal is a yellow liquid, slightly denser than water, boiling at 104 ℃, insoluble in water, readily soluble in alcohol and most non-volatile oils. The chicken essence has strong fragrance characteristics of chicken fragrance and chicken oil, is a food spice allowed to be used by national standard, and is mainly used for preparing chicken essence.
2, 4-decadienal is not only a main component of the chicken oily essence, but also a substance exhibiting a strong chicken fat flavor as a main characteristic. Therefore, the method can be used as a marker for determining the embedding rate of the chicken essence microcapsules, and no method for extracting 2, 4-decadienal from the microcapsules is available at present.
Disclosure of Invention
The invention aims to provide a method for extracting, analyzing and detecting 2, 4-decadienal.
The technical scheme adopted by the invention is as follows:
the invention provides a method for extracting 2, 4-decadienal, which comprises the following steps:
accurately weighing 0.2g of powder microcapsule containing 2, 4-decadienal, placing the powder microcapsule into a 10mL centrifuge tube, sucking 2mL of water by using a 1mL pipette to dissolve the powder microcapsule, adding 4mL of organic solvent after dissolving, carrying out ultrasonic treatment for 1min, standing for 2min to stratify, sucking 1mL of supernatant, adding 0.2g of anhydrous sodium sulfate, standing for 12h, and then passing through a membrane (0.22um organic filter membrane), thus obtaining the liquid to be detected.
Preferably, the organic solvent is n-hexane, petroleum ether, chloroform or diethyl ether. More preferably diethyl ether.
The invention also provides an analysis and detection method of 2, 4-decadienal, which comprises the following steps:
(1) extraction of 2, 4-decadienal:
accurately weighing 0.2g of powder microcapsule containing 2, 4-decadienal, placing the powder microcapsule into a 10mL centrifuge tube, sucking 2mL of water by using a 1mL pipette to dissolve the powder microcapsule, adding 4mL of organic solvent after dissolving, carrying out ultrasonic treatment for 1min, standing for 2min to stratify, sucking 1mL of supernatant, adding 0.2g of anhydrous sodium sulfate, standing for 12h, and then passing through a membrane (0.22um organic filter membrane), thus obtaining a solution to be detected;
(2) GC detection of 2, 4-decadienal
Placing the solution to be measured in the step (1) into a sample bottle, screwing a sealing cover, and measuring the sample under the following measuring conditions:
hp-5 capillary column (60m × 0.25mm × 0.25 μm), injection inlet temperature 250 deg.C, carrier gas is high-purity (greater than or equal to 99.999%) helium, carrier gas flow rate is 1.0mL/min, temperature programming: the initial temperature is 40 ℃, the temperature is kept for 2.0min, the temperature is increased to 250 ℃ at the speed of 10 ℃/min, and the temperature is kept for 10.0 min;
an EI ion source; electron energy 70 eV; the temperature of the four-level bar is 150 ℃, and the interface temperature is 260 ℃; electron multiplier voltage 1423V; the ion source temperature is 230 ℃; tuning in a standard manner; selecting a full scanning mode, wherein the mass scanning range is as follows: 40-400 amu, solvent delay 10 min.
Preferably, the organic solvent is n-hexane, petroleum ether, chloroform or diethyl ether. More preferably diethyl ether.
The invention has the following beneficial effects:
the invention provides a method for extracting, analyzing and detecting 2, 4-decadienal, which is simple and has small error.
Drawings
FIG. 1 is a standard curve for 2, 4-decadienal.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1
A method for measuring 2, 4-decadienal in essence powder comprises the following steps:
(1) extraction of 2, 4-decadienal:
accurately weighing 0.2g of powder microcapsule containing 2, 4-decadienal, placing the powder microcapsule into a 10mL centrifuge tube, sucking 2mL of water by using a 1mL pipette to dissolve the powder microcapsule, adding 4mL of diethyl ether after dissolving, carrying out ultrasonic treatment for 1min, standing for 2min to stratify, sucking 1mL of supernatant, adding 0.2g of anhydrous sodium sulfate, standing for 12h, and then passing through a membrane (0.22um organic filter membrane), thus obtaining a solution to be detected; (2) GC detection of 2, 4-decadienal
Placing the solution to be measured in the step (1) into a sample bottle, screwing a sealing cover, and measuring the sample under the following measuring conditions:
hp-5 capillary column (60m × 0.25mm × 0.25 μm), injection inlet temperature 250 deg.C, carrier gas is high-purity (greater than or equal to 99.999%) helium, carrier gas flow rate is 1.0mL/min, temperature programming: the initial temperature is 40 ℃, the temperature is kept for 2.0min, and the temperature is increased to 250 ℃ at the temperature of 10 ℃/min and kept for 10.0 min.
An EI ion source; electron energy 70 eV; the temperature of the four-level bar is 150 ℃, and the interface temperature is 260 ℃; electron multiplier voltage 1423V; the ion source temperature is 230 ℃; tuning in a standard manner; selecting a full scanning mode, wherein the mass scanning range is as follows: 40-400 amu, solvent delay 10 min.
Determination of the recovery of the different organic solvents:
preparation of comparative sample:
accurately weighing 0.2g of powder microcapsule containing 2, 4-decadienal, placing the powder microcapsule into a 10mL centrifuge tube, adding 0.03g of 2, 4-decadienal monomer, absorbing 2mL of water by using a 1mL pipette to dissolve the monomer, adding 4mL of organic solvent after dissolving, carrying out ultrasonic treatment for 1min, standing for 2min to stratify, absorbing 1mL of supernatant, adding 0.2g of anhydrous sodium sulfate, standing for 12h, and then passing through a membrane (an organic filter membrane of 0.22 um) to obtain a sample to be detected;
blank control sample preparation:
accurately weighing 0.2g of powder microcapsule containing 2, 4-decadienal, placing the powder microcapsule into a 10mL centrifuge tube, sucking 2mL of water by using a 1mL pipette to dissolve the powder microcapsule, adding 4mL of organic solvent after dissolving, carrying out ultrasonic treatment for 1min, standing for 2min to stratify, sucking 1mL of supernatant, adding 0.2g of anhydrous sodium sulfate, standing for 12h, and then passing through a membrane (an organic filter membrane of 0.22 um), thus obtaining a sample to be detected;
the results of the measurement were as follows:
when the organic solvent is diethyl ether, the results are as follows:
the results of the measurements of the extraction of 2, 4-decadienal from the samples with different organic solvents are shown in the following table:
as can be seen from the above table, the extraction rate of diethyl ether to 2, 4-decadienal in the microcapsule is the highest, so diethyl ether can be selected as the best extraction solvent for 2, 4-decadienal.
And (3) preparing a standard curve:
accurately weighing 0.36g of 2, 4-decadienal monomer, placing the monomer into a 10mL centrifuge tube, sucking 10mL of diethyl ether by a pipette, dissolving the diethyl ether, oscillating for 2min by a vortex oscillator to obtain an initial standard solution with the concentration of 36mg/mL, and sequentially diluting the prepared standard solution in different gradients, wherein the diluted concentrations are as follows: 12mg/mL, 6mg/mL, 2mg/mL, 1mg/mL, and the standard curve of the measurement is shown in FIG. 1.
And (3) repeatability experiment:
the sample extraction method is shown in (1), and a gas phase analyzer is adopted to continuously sample the same prepared sample for 6 times, wherein RSD (percent) is 1.91 percent.
And (3) precision experiment:
the same sample was extracted in the same manner as in (1), and extraction was repeated six times, and the RSD (%) was 2.23% by sampling. Stability:
the same prepared sample was measured every 6 hours until 30 hours, and RSD (%) was 1.32% by sample injection.
Claims (1)
1. The method for analyzing and detecting the 2, 4-decadienal is characterized by comprising the following steps: the method comprises the following steps:
(1) extraction of 2, 4-decadienal:
accurately weighing 0.2g of powder microcapsule containing 2, 4-decadienal, placing the powder microcapsule into a 10mL centrifuge tube, sucking 2mL of water by using a 1mL pipette to dissolve the powder microcapsule, adding 4mL of organic solvent after dissolving, carrying out ultrasonic treatment for 1min, standing for 2min to stratify, sucking 1mL of supernatant, adding 0.2g of anhydrous sodium sulfate, standing for 12h, and then passing through a 0.22 mu m organic filter membrane to obtain a solution to be detected;
(2) GC detection of 2, 4-decadienal
Placing the solution to be measured in the step (1) into a sample bottle, screwing a sealing cover, and measuring the sample under the following measuring conditions:
hp-5 capillary column, 60m × 0.25mm × 0.25 μm, injection inlet temperature 250 deg.C, carrier gas of high-purity helium gas greater than or equal to 99.999%, carrier gas flow rate of 1.0mL/min, temperature programming: the initial temperature is 40 ℃, the temperature is kept for 2.0min, the temperature is increased to 250 ℃ at the speed of 10 ℃/min, and the temperature is kept for 10.0 min;
an EI ion source; electron energy 70 eV; the temperature of the four-level bar is 150 ℃, and the interface temperature is 260 ℃; electron multiplier voltage 1423V; the ion source temperature is 230 ℃; tuning in a standard manner; selecting a full scanning mode, wherein the mass scanning range is as follows: 40-400 amu, and delaying the solvent for 10 min;
the organic solvent is diethyl ether.
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| CN201610625089.XA CN106248827B (en) | 2016-07-28 | 2016-07-28 | Extraction and detection method of 2, 4-decadienal |
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