CN106248827A - The extraction of a kind of 2,4 decadienals and detection method - Google Patents
The extraction of a kind of 2,4 decadienals and detection method Download PDFInfo
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- CN106248827A CN106248827A CN201610625089.XA CN201610625089A CN106248827A CN 106248827 A CN106248827 A CN 106248827A CN 201610625089 A CN201610625089 A CN 201610625089A CN 106248827 A CN106248827 A CN 106248827A
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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
- G01N30/04—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
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas 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
- 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
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
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Abstract
The present invention relates to a kind of 2, the extraction of 4 decadienals and detection method, extracting method of the present invention comprises the steps: that accurately weighing 0.2g contains 2, the powder microcapsule of 4 decadienals is placed in the centrifuge tube of 10mL, dissolved with 1mL pipette, extract 2mL water afterwards, after to be dissolved, add 4mL organic solvent, ultrasonic 1min, stand 2min to wait to be layered, Aspirate supernatant 1mL, and add 0.2g anhydrous sodium sulfate, cross film (organic filter membrane of 0.22um) after standing 12h, be liquid to be measured.The inventive method is simple, and error is little.
Description
Technical field
The present invention relates to a kind of detection method, measure 2 particularly to one, the method for 4-decadienal.
Background technology
2,4-decadienals are kind of yellow liquids, and density is slightly more than water, and boiling point 104 DEG C is water insoluble, is soluble in ethanol
With most of nonvolatile oils.Have that strong chicken is fragrant and the odor characteristic of chicken oil, national regulations its be the food allowing use
With spice, it is mainly used in configuring in chicken essence.
2,4-decadienals are not only the main component of chicken meat oily essence, and are to present strong chicken fat local flavor principal character
Material.Therefore, as a mark of the mensuration microcapsule embedded rate of chicken essence, and can there are no at present about from micro-glue
The method extracting 2,4-decadienal in capsule.
Summary of the invention
It is an object of the invention to provide extraction and the analyzing detecting method of a kind of 2,4-decadienal.
The technical solution used in the present invention is:
The invention provides a kind of 2, the extracting method of 4-decadienal, the method comprises the steps:
Accurately weighing 0.2g and contain 2, the powder microcapsule of 4-decadienal is placed in the centrifuge tube of 10mL, after use 1mL
Pipette, extract 2mL water is dissolved, to be dissolved after, add 4mL organic solvent, ultrasonic 1min, stand 2min and wait to be layered, inhale
Take supernatant 1mL, and add 0.2g anhydrous sodium sulfate, cross film (organic filter membrane of 0.22um) after standing 12h, be liquid to be measured.
Preferably, described organic solvent is normal hexane, petroleum ether, chloroform or ether.More preferably ether.
Present invention also offers a kind of 2, the analyzing detecting method of 4-decadienal, the method comprises the steps:
(1) extraction of 2,4-decadienal:
Accurately weighing 0.2g and contain 2, the powder microcapsule of 4-decadienal is placed in the centrifuge tube of 10mL, after use 1mL
Pipette, extract 2mL water is dissolved, to be dissolved after, add 4mL organic solvent, ultrasonic 1min, stand 2min and wait to be layered, inhale
Take supernatant 1mL, and add 0.2g anhydrous sodium sulfate, cross film (organic filter membrane of 0.22um) after standing 12h, be liquid to be measured；
(2) the GC detection of 2,4-decadienal
Being placed in sample bottle by liquid to be measured in step (1), screwing hermetic lid, carry out test sample, condition determination is as follows:
Hp-5 capillary column (60m × 0.25mm × 0.25 μm), injector temperature 250 DEG C, carrier gas be high-purity (>=
99.999%) helium, flow rate of carrier gas is 1.0mL/min, temperature programming: initial temperature 40 DEG C, keeps 2.0min, 10 DEG C/min liter
10.0min is kept to 250 DEG C；
EI ion source；Electron energy 70eV；Level Four bar temperature 150 DEG C, interface temperature 260 DEG C；Electron multiplier voltage
1423V；Ion source temperature 230 DEG C；Employing standard mode tunes；Select full scan pattern, mass scan range: 40～
400amu, solvent delay 10min.
Preferably, described organic solvent is normal hexane, petroleum ether, chloroform or ether.More preferably ether.
The present invention is had the advantages that
The present invention provides a kind of 2, and the extraction of 4-decadienal and analyzing detecting method, the inventive method is simple, and error is little.
Accompanying drawing explanation
Fig. 1 is the standard curve of 2,4-decadienal.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, but does not limit protection scope of the present invention.
Embodiment 1
A kind of measure in essence powder 2, the method for 4-decadienal, comprise the steps:
(1) extraction of 2,4-decadienal:
Accurately weighing 0.2g and contain 2, the powder microcapsule of 4-decadienal is placed in the centrifuge tube of 10mL, after use 1mL
Pipette, extract 2mL water is dissolved, to be dissolved after, add the ultrasonic 1min of 4mL ether, stand 2min and wait to be layered, in absorption
Clear liquid 1mL, and add 0.2g anhydrous sodium sulfate, cross film (organic filter membrane of 0.22um) after standing 12h, be liquid to be measured；(2)2,
The GC detection of 4-decadienal
Being placed in sample bottle by liquid to be measured in step (1), screwing hermetic lid, get final product test sample, condition determination is as follows:
Hp-5 capillary column (60m × 0.25mm × 0.25 μm), injector temperature 250 DEG C, carrier gas be high-purity (>=
99.999%) helium, flow rate of carrier gas is 1.0mL/min, temperature programming: initial temperature 40 DEG C, keeps 2.0min, 10 DEG C/min liter
10.0min is kept to 250 DEG C.
EI ion source；Electron energy 70eV；Level Four bar temperature 150 DEG C, interface temperature 260 DEG C；Electron multiplier voltage
1423V；Ion source temperature 230 DEG C；Employing standard mode tunes；Select full scan pattern, mass scan range: 40～
400amu, solvent delay 10min.
The response rate of mensuration different organic solvents:
Prepared by comparative sample:
Accurately weighing 0.2g and contain 2, the powder microcapsule of 4-decadienal is placed in the centrifuge tube of 10mL, and adds
The 2 of 0.03g, 4-decadienal monomer, rear dissolved with 1mL pipette, extract 2mL water, to be dissolved after, add 4mL organic
Solvent, ultrasonic 1min, stand 2min and wait to be layered, Aspirate supernatant 1mL, and add 0.2g anhydrous sodium sulfate, cross film after standing 12h
(organic filter membrane of 0.22um), is and treats test sample；
Prepared by blank control sample:
Accurately weighing 0.2g and contain 2, the powder microcapsule of 4-decadienal is placed in the centrifuge tube of 10mL, then moves with 1mL
Liquid pipe is drawn 2mL water and is dissolved, to be dissolved after, add 4mL organic solvent, ultrasonic 1min, stand 2min and wait to be layered, absorption
Supernatant 1mL, and add 0.2g anhydrous sodium sulfate, cross film (organic filter membrane of 0.22um) after standing 12h, be and treat test sample；
Measurement result is as follows:
When organic solvent selects ether, result is as follows:
Different organic solvents is as shown in the table for the measurement result of the extraction ratio of 2,4-decadienal in sample:
As can be seen from the above table, ether is for 2 in microcapsule, and the extraction ratio of 4-decadienal is the highest, therefore can select
Select the ether optimum extraction solvent as 2,4-decadienal.
The making of standard curve:
Accurately weigh 0.36g2,4-decadienal monomer to be placed in 10mL centrifuge tube, then with pipette, extract 10mL ether,
Dissolved, vibrate 2min with turbula shaker, obtain the primary standard liquid that concentration is 36mg/mL, and successively to above-mentioned configuration
The dilution of different gradient made by good titer, and the concentration after dilution is followed successively by: 12mg/mL, 6mg/mL, 2mg/mL, 1mg/mL, surveys
Fixed standard curve is as shown in Figure 1.
Repeated experiment:
Sample extraction method as shown in (1), use gas phase analysis device to the same sample continuous sample introduction prepared 6 times,
RSD (%)=1.91%.
Precision Experiment:
Same sample, sample extraction method, as shown in (1), repeats to extract six times, and sample introduction measures, RSD (%)=2.23%.
Stability:
The sample preparing same portion measured once every 6 hours, measures and stops to 30h, and sample introduction measures, and RSD (%)=
1.32%.
Claims (6)
1. one kind 2, the extracting method of 4-decadienal, it is characterised in that: the method comprises the steps:
Accurately weighing 0.2g and contain 2, the powder microcapsule of 4-decadienal is placed in the centrifuge tube of 10mL, after move liquid with 1mL
Pipe is drawn 2mL water and is dissolved, to be dissolved after, add 4mL organic solvent, ultrasonic 1min, standing 2min wait to be layered, in absorption
Clear liquid 1mL, and add 0.2g anhydrous sodium sulfate, cross film (organic filter membrane of 0.22um) after standing 12h, be liquid to be measured.
The most according to claim 1 a kind of 2, the extracting method of 4-decadienal, it is characterised in that: described organic solvent is
Normal hexane, petroleum ether, chloroform or ether.
The most according to claim 2 a kind of 2, the extracting method of 4-decadienal, it is characterised in that: described organic solvent is
Ether.
4. one kind 2, the analyzing detecting method of 4-decadienal, it is characterised in that: the method comprises the steps:
(1) extraction of 2,4-decadienal:
Accurately weighing 0.2g and contain 2, the powder microcapsule of 4-decadienal is placed in the centrifuge tube of 10mL, after move liquid with 1mL
Pipe is drawn 2mL water and is dissolved, to be dissolved after, add 4mL organic solvent, ultrasonic 1min, standing 2min wait to be layered, in absorption
Clear liquid 1mL, and add 0.2g anhydrous sodium sulfate, cross film (organic filter membrane of 0.22um) after standing 12h, be liquid to be measured；
(2) the GC detection of 2,4-decadienal
Being placed in sample bottle by liquid to be measured in step (1), screwing hermetic lid, carry out test sample, condition determination is as follows:
Hp-5 capillary column (60m × 0.25mm × 0.25 μm), injector temperature 250 DEG C, carrier gas is high-purity (>=99.999%)
Helium, flow rate of carrier gas is 1.0mL/min, temperature programming: initial temperature 40 DEG C, keeps 2.0min, 10 DEG C/min to rise to 250 DEG C of guarantors
Hold 10.0min；
EI ion source；Electron energy 70eV；Level Four bar temperature 150 DEG C, interface temperature 260 DEG C；Electron multiplier voltage 1423V；
Ion source temperature 230 DEG C；Employing standard mode tunes；Select full scan pattern, mass scan range: 40～400amu, solvent
Postpone 10min.
The most according to claim 4 a kind of 2, the analyzing detecting method of 4-decadienal, it is characterised in that: described is organic
Solvent is normal hexane, petroleum ether, chloroform or ether.
The most according to claim 5 a kind of 2, the analyzing detecting method of 4-decadienal, it is characterised in that: described is organic
Solvent is 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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| CN201610625089.XA CN106248827B (en) | 2016-07-28 | 2016-07-28 | Extraction and detection method of 2, 4-decadienal |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109633064A (en) * | 2018-12-28 | 2019-04-16 | 无限极（中国）有限公司 | A method of using 2,4- diene aldehyde compound in GC-MS measurement daily essence |
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- 2016-07-28 CN CN201610625089.XA patent/CN106248827B/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109633064A (en) * | 2018-12-28 | 2019-04-16 | 无限极（中国）有限公司 | A method of using 2,4- diene aldehyde compound in GC-MS measurement daily essence |
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Effective date of registration: 20191225 Address after: 300300 No. 11 Li Bei Road, Dongli Economic Development Zone, Tianjin Applicant after: Tianjin Chunfa Biotechnology Group Co., Ltd. Address before: 300300 No. 30, two weft Road, Dongli Economic Development Zone, Tianjin, China Applicant before: Tianjin Chunsheng Halal Foods Co., Ltd. |
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