CN106442601B - A kind of method of lipid oxidation in quick detection meat cold storage procedure - Google Patents
A kind of method of lipid oxidation in quick detection meat cold storage procedure Download PDFInfo
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- CN106442601B CN106442601B CN201611193628.3A CN201611193628A CN106442601B CN 106442601 B CN106442601 B CN 106442601B CN 201611193628 A CN201611193628 A CN 201611193628A CN 106442601 B CN106442601 B CN 106442601B
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- 238000000034 method Methods 0.000 title claims abstract description 48
- 235000013372 meat Nutrition 0.000 title claims abstract description 39
- 238000001514 detection method Methods 0.000 title claims abstract description 33
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 29
- 230000003647 oxidation Effects 0.000 title claims abstract description 28
- 150000002632 lipids Chemical class 0.000 title claims abstract description 22
- 238000003860 storage Methods 0.000 title claims abstract description 17
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 74
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000004435 EPR spectroscopy Methods 0.000 claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 32
- 239000011259 mixed solution Substances 0.000 claims abstract description 25
- 239000003708 ampul Substances 0.000 claims abstract description 18
- 239000010453 quartz Substances 0.000 claims abstract description 18
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims abstract description 18
- 238000005119 centrifugation Methods 0.000 claims abstract description 10
- 238000005057 refrigeration Methods 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 230000010355 oscillation Effects 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- WORJEOGGNQDSOE-UHFFFAOYSA-N chloroform;methanol Chemical compound OC.ClC(Cl)Cl WORJEOGGNQDSOE-UHFFFAOYSA-N 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- QDYBCIWLGJMJGO-UHFFFAOYSA-N dinitromethanone Chemical compound [O-][N+](=O)C(=O)[N+]([O-])=O QDYBCIWLGJMJGO-UHFFFAOYSA-N 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 8
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 6
- 238000011534 incubation Methods 0.000 claims description 5
- 230000001186 cumulative effect Effects 0.000 claims description 4
- RNRMWTCECDHNQU-XYOKQWHBSA-N N-tert-butyl-1-(1-oxidopyridin-1-ium-4-yl)methanimine oxide Chemical compound CC(C)(C)[N+](\[O-])=C/C1=CC=[N+]([O-])C=C1 RNRMWTCECDHNQU-XYOKQWHBSA-N 0.000 abstract description 9
- 238000012360 testing method Methods 0.000 abstract description 4
- -1 oxygen radical Chemical class 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- 235000013305 food Nutrition 0.000 description 4
- 239000002957 persistent organic pollutant Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 150000003254 radicals Chemical class 0.000 description 4
- 235000015278 beef Nutrition 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 235000015277 pork Nutrition 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- 241000287828 Gallus gallus Species 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 235000013622 meat product Nutrition 0.000 description 2
- 230000001404 mediated effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- RVBUGGBMJDPOST-UHFFFAOYSA-N 2-thiobarbituric acid Chemical compound O=C1CC(=O)NC(=S)N1 RVBUGGBMJDPOST-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001212 derivatisation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 235000003642 hunger Nutrition 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000003859 lipid peroxidation Effects 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000004792 oxidative damage Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- BHAAPTBBJKJZER-UHFFFAOYSA-N p-anisidine Chemical compound COC1=CC=C(N)C=C1 BHAAPTBBJKJZER-UHFFFAOYSA-N 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000013319 spin trapping Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/10—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using electron paramagnetic resonance
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- Physics & Mathematics (AREA)
- High Energy & Nuclear Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses a kind of method of lipid oxidation in quick detection meat cold storage procedure, step are as follows：1, take the meat sample after the refrigeration of constant weight；2, it is incubated after adding POBN solution into sample；3, chloroform and methanol mixed solution and deionized water are added into step 2 system；4, step 3 system is homogenized；5, chloroform and methanol mixed solution are added into step 4 system；6, in the system of oscillation step 5；7, then step 6 system is centrifuged；8, chloroform layer is separated from the system after centrifugation；9, isolated chloroformic solution is collected after sodium peroxydisulfate post；10, the chloroformic solution rotary evaporation in collection step 9 removes chloroform；11, the sample in collection step 10 after rotary evaporation, it is put into electron spin resonance detection quartz ampoule；12, quartz ampoule is put into electron spin resonanceapparatus and detected.It is short that there is this hair each sample detection to take, convenient rapid；The advantages of testing result is accurate.
Description
Technical field
The invention belongs to meat product technical field of quality detection, more particularly to a kind of quick detection meat cold storage procedure
The method of middle lipid oxidation.
Background technology
Chilled Meats with its security, trophism and better than traditional chilled meat, Fresh meat, as fresh meat consumption must
Right trend.But in Chilled Meats processing, circulation and storage, inevitably by temperature, light, ray, oxygen, moisture and urge
The influence of the external environments such as agent, these factors can aoxidize the fat of meat in itself, produce the compounds such as aldehyde, alcohol, ketone, production
Raw offensive odour, bitter taste, reduce the quality and nutritive value of meat, while can also cause the brown stain of meat surface, can
Acceptance is also greatly reduced, so as to cause very big loss.Some toxic compounds can be produced when aoxidizing serious, jeopardize human body
Health even life.
Test result indicates that：Why food can be corrupt, in addition to bacterium infection, is primarily due to anti-there occurs oxidation
Should, the food containing grease, particularly meat product are easy to occur the lipid oxidation reaction of free radical mediated.Its mediated process
As shown in Figure 4.
ESR (electron spin resonance) technology is particularly suitable for determining various free radicals, for active oxygen radical
The method that detection can use spin trapping.Agent for capturing ST and free radical R, which reacts the spin adduct R-ST to be formed, has phase
To the longer life-span and there are the ESR POPs of feature, easily can be detected on the instrument of ESR POPs.Active oxygen radical is being eaten
Conclusive effect is played in the oxydative spoilage of product.When making quality control, can periodically it be added in the flow of food production
Capturing agent, timing sampling, then detected on the instrument of ESR POPs.It is used as Product checking or research, can be first using pressure
Property measure cause oxidative damage, such as heat illumination or irradiation, and add agent for capturing in the sample and carry out ESR detections.
Caused primary and secondary during detection lipid oxidation is focused primarily upon to the detection method of lipid oxidation at present
Oxidation product is so as to reacting degree of oxidation.Detection method for oxidation primary product is mainly：Peroxide value method, the method are adopted
With titration by color change so that it is determined that reaction end, the color of sample has very big interference to result, while is not suitable for full
The high sample with content of fatty acid.Infra-red sepectrometry, although the method can accurately react degree of oxidation, complex operation, and
Cost is higher.Gas chromatography, the method derivatization treatment of sample before gas chromatographic analysis is carried out may cause insatiable hunger
Change with sample physical property, so as to bring detection error.Liquid chromatography, the method equally operate it is relatively complicated, while when detecting
Between it is longer.Mainly there are acid value, thiobarbituric acid reaction thing determination method, anisidine value for the detection method of secondary oxidative product
Method, electrical conductivity method, fluorescence method, gas chromatography etc., but these methods are limited to color sample and influenceed greatly, cumbersome, by-product
Thing has an impact to testing result.
The content of the invention
It is an object of the invention to provide a kind of method of lipid oxidation in quick detection meat cold storage procedure.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：Lipid oxygen in a kind of quick detection meat cold storage procedure
The method of change, comprises the following steps：
Step 1, the meat sample after the refrigeration of constant weight is taken；Preferably, in step 1, the weight of meat sample is 0.5
~2g.
Step 2, it is incubated after adding a- (4- pyridine radicals -1- oxygen)-N- tert-butyl group nitroketone solution into sample；It is preferred that
Ground, in step 2, the concentration of a- (4- pyridine radicals -1- oxygen)-N- tert-butyl group nitroketone solution is 0.1~200mM, volume is 1~
4ml；Incubation time is 10~60min, and incubation temperature is 0 DEG C.
Step 3, chloroform and methanol mixed solution and deionized water are added into step 2 system；Preferably, in step 3,
In step 3, the chloroform and the volume ratio of the two in methanol mixed solution are 1:1-5:1, chloroform methanol mixed solution is overall
Product is 1~10ml, and the addition of deionized water is 1~8ml.
Step 4, step 3 system is homogenized；
Step 5, chloroform and methanol mixed solution are added into step 4 system；Preferably, in steps of 5, the chloroform with
The ratio of the two in methanol mixed solution is 1:1-5:1, chloroform methanol mixed solution cumulative volume is 10~40ml.
Step 6, the system of oscillation step 5 on turbula shaker；Preferably, in step 6, the vortex oscillation time is
2~5min.
Step 7, then step 6 system is centrifuged；Preferably, in step 7, the centrifugal force be 500~
1000g, centrifugation time are 5~15min.
Step 8, chloroform layer is separated from the system after centrifugation；Preferably, in step 8, separatory funnel is utilized
Chloroform layer is separated from the system after centrifugation.
Step 9, isolated chloroformic solution is collected after sodium peroxydisulfate post；Sodium sulphate post plays dry effect can be with
Moisture is absorbed, chloroform recovery solution is further purified.
Step 10, the chloroformic solution rotary evaporation in collection step 9 removes chloroform；Preferably, in step 10, the rotation
Turn evaporating temperature as 30~70 DEG C.
Step 11, the sample in collection step 10 after rotary evaporation, it is put into electron spin resonance detection quartz ampoule；
Step 12, quartz ampoule is put into electron spin resonanceapparatus and detected.Preferably, in electron spin resonanceapparatus
Core field intensity is 3500G, microwave power 1.86mW, microwave frequency 9.85GHz, and multiplication factor is 1.00 × 106, modulation
Amplitude is 1.00G, modulating frequency 100kHz, time constant 240ms, sweep time 245.76s.
The beneficial effects of the invention are as follows：
The method that this hair detects lipid oxidation in meat frozen storage based on ESR methods, each sample detection take short, side
Just it is rapid；Testing result is accurate.
The advantages of ESR POPs method that compares is：1st, accurate reliable, selectivity is strong；2nd, time saving to be afraid of, efficiently, quickly, sample is not
Need separation or the again complicated processes such as processing；3rd, it can realize that automatic batch detects, simplify measurement process and reduction work is strong
Degree；4th, it is cheap using POBN agent for capturing, cost；5th, it is a kind of measuring method of physics, sample is not damaged.
Brief description of the drawings
Fig. 1 is the feature peak type based on lipid oxidation situation in the beef of ESR technology for detection embodiment 2；
Fig. 2 is the feature peak type based on lipid oxidation situation in the pork of ESR technology for detection embodiment 3；
Fig. 3 is the feature peak type based on lipid oxidation situation in the chicken of ESR technology for detection embodiment 4；
Fig. 4 is the schematic diagram of oils food lipid peroxidation process.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, unreceipted actual conditions in embodiment
Person, the condition suggested according to normal condition or manufacturer are carried out.Agents useful for same or the unreceipted production firm person of instrument, being can be with
Pass through the conventional products of acquisition purchased in market.
The method of lipid oxidation comprises the following steps in a kind of quick detection meat cold storage procedure of embodiment：
Step 1, the meat sample after the refrigeration of constant weight is taken；Because the detection of electron spin resonanceapparatus only needs on a small quantity
Sample, so in a preferred embodiment, the weight of meat sample is 0.5~2g.
Step 2, a- (4- pyridine radicals -1- oxygen)-N- tert-butyl group nitroketones (POBN, CAS66893-81- is added into sample
0) it is incubated after solution；Preferably, in step 2, the concentration of a- (4- pyridine radicals -1- oxygen)-N- tert-butyl group nitroketone solution is
0.1~200mM, volume are 1~4ml；Incubation time is 10~60min, and incubation temperature is 0 DEG C.
Step 3, chloroform and methanol mixed solution and deionized water are added into step 2 system；Preferably, in step 3,
In step 3, the chloroform and the volume ratio of the two in methanol mixed solution are 1:1-5:1, chloroform methanol mixed solution is overall
Product is 1~10ml, and the addition of deionized water is 1~8ml.
Step 4, step 3 system is homogenized；
Step 5, chloroform and methanol mixed solution are added into step 4 system；Preferably, in steps of 5, the chloroform with
The ratio of the two in methanol mixed solution is 1:1-5:1, chloroform methanol mixed solution cumulative volume is 10~40ml.
Step 6, the system of oscillation step 5 on turbula shaker；Preferably, in step 6, the vortex oscillation time is
2~5min.
Step 7, then step 6 system is centrifuged；Preferably, in step 7, the centrifugal force be 500~
1000g, centrifugation time are 5~15min.
Step 8, chloroform layer is separated from the system after centrifugation；Preferably, in step 8, separatory funnel is utilized
Chloroform layer is separated from the system after centrifugation.
Step 9, isolated chloroformic solution is collected after sodium peroxydisulfate post；Sodium sulphate post plays dry effect can be with
Moisture is absorbed, chloroform recovery solution is further purified.
Step 10, the chloroformic solution rotary evaporation in collection step 9 removes chloroform；Preferably, in step 10, the rotation
Turn evaporating temperature as 30~70 DEG C.
Step 11, the sample in collection step 10 after rotary evaporation, it is put into electron spin resonance detection quartz ampoule；
Step 12, quartz ampoule is put into electron spin resonanceapparatus and detected.Preferably, in electron spin resonanceapparatus
Core field intensity is 3500G, microwave power 1.86mW, microwave frequency 9.85GHz, and multiplication factor is 1.00 × 106, modulation
Amplitude is 1.00G, modulating frequency 100kHz, time constant 240ms, sweep time 245.76s.
Agents useful for same, the specifications and models of instrument and manufacturer are as follows in following examples：
POBN (a- (4- pyridine radicals -1- oxygen)-N- tert-butyl groups nitroketone), Japanese TCI Reagent Companies, purity 98%.It is vortexed
Oscillator, Industrial Co., Ltd. of upper Nereid section, model：XW-80A.Centrifuge, Hitachi, Ltd's model：CF 16RXⅡ；Sodium sulphate
Post, Agilent company, model：Straight pipe type post 15g, 60mL.
Embodiment 1
Take the beef 0.5g of refrigeration 3 days；
1ml is added into meat, 80mM POBN (a- (4- pyridine radicals -1- oxygen)-N- tert-butyl groups nitroketone) solution is carried out
It is incubated, is incubated 20min；
8ml chloroform methanols are added into above-mentioned system and mix molten, volume ratio 1:1 and 6ml deionized waters；
Above-mentioned system is homogenized；
Add 15ml chloroform methanol mixed solutions again into above-mentioned system, the two volume ratio is 1:1；
Above-mentioned system 2min is vibrated on turbula shaker；
8min is then centrifuged to above-mentioned system with 500g centrifugal force；
Chloroform layer is separated from system with separatory funnel：
Chloroformic solution is collected after sodium peroxydisulfate pillar；
The above-mentioned chloroformic solution rotary evaporation removal chloroform crossed after pillar is collected, rotating evaporation temperature is 50 DEG C；
The sample after above-mentioned rotary evaporation is collected, ESR is put into and detects in special quartz ampoule；
Quartz ampoule is put into ESR resonators, detected, ESR central magnetic field intensity is 3500G, and microwave power is
1.86mW, microwave frequency 9.85GHz, multiplication factor are 1.00 × 106, modulation amplitude 1.00G；Modulating frequency is
100kHz；Time constant is 240ms；Sweep time is 245.76s, and its peak height value is 0.243 × 106。
Free radical forms the peak height of feature peak type after the meat oxidation that ESR is detected and positive is presented in meat degree of oxidation
Close, meat degree of oxidation is more serious, and the peak height with the characteristic peak detected on ESR is also higher.
Embodiment 2
Take the beef 1g of refrigeration 5 days；
1.5ml is added into meat, 70mM POBN solution is incubated, and is incubated 40min；
6ml chloroform methanols are added into above-mentioned system and mix molten, volume ratio 4:1 and 5ml deionized waters；
Above-mentioned system is homogenized；
Add 18ml chloroform methanol mixed solutions again into above-mentioned system, the two volume ratio is 4:1；
Above-mentioned system 2.5min is vibrated on turbula shaker；
10min is then centrifuged to above-mentioned system with 800g centrifugal force；
Chloroform layer is separated from system with separatory funnel：
Chloroformic solution is collected after sodium peroxydisulfate pillar；
The above-mentioned chloroformic solution rotary evaporation removal chloroform crossed after pillar is collected, rotating evaporation temperature is 55 DEG C；
The sample after above-mentioned rotary evaporation is collected, ESR is put into and detects in special quartz ampoule；
Quartz ampoule is put into ESR resonators, detected, ESR central magnetic field intensity is 3500G, and microwave power is
1.86mW, microwave frequency 9.85GHz, multiplication factor are 1.00 × 106, modulation amplitude 1.00G；Modulating frequency is
100kHz；Time constant is 240ms；Sweep time is 245.76s, and its peak height value is 0.495 × 106。
Embodiment 3
Take the pork 1g of refrigeration 5 days；
2ml is added into meat, 50mM POBN solution is incubated, and is incubated 30min；
10ml chloroform methanols are added into above-mentioned system and mix molten, volume ratio 3:1 and 4ml deionized waters；
Above-mentioned system is homogenized；
Add 30ml chloroform methanol mixed solutions again into above-mentioned system, the two volume ratio is 3:1；
Above-mentioned system 3min is vibrated on turbula shaker；
15min is then centrifuged to above-mentioned system with 800g centrifugal force；
Chloroform layer is separated from system with separatory funnel：
Chloroformic solution is collected after sodium peroxydisulfate pillar；
The above-mentioned chloroformic solution rotary evaporation removal chloroform crossed after pillar is collected, rotating evaporation temperature is 45 DEG C；
The sample after above-mentioned rotary evaporation is collected, ESR is put into and detects in special quartz ampoule；
Quartz ampoule is put into ESR resonators, detected, ESR central magnetic field intensity is 3500G, and microwave power is
1.86mW, microwave frequency 9.85GHz, multiplication factor are 1.00 × 106, modulation amplitude 1.00G；Modulating frequency is
100kHz；Time constant is 240ms；Sweep time is 245.76s, and its peak height value is 0.386 × 106。
Embodiment 4
Take the chicken 1g of refrigeration 7 days；
1ml is added into meat, 100mM POBN solution is incubated, and is incubated 50min；
6ml chloroform methanols are added into above-mentioned system and mix molten, volume ratio 2:1 and 4ml deionized waters；
Above-mentioned system is homogenized；
Add 20ml chloroform methanol mixed solutions again into above-mentioned system, the two volume ratio is 2:1；
Above-mentioned system 2min is vibrated on turbula shaker；
10min is then centrifuged to above-mentioned system with 800g centrifugal force；
Chloroform layer is separated from system with separatory funnel：
Chloroformic solution is collected after sodium peroxydisulfate pillar；
The above-mentioned chloroformic solution rotary evaporation removal chloroform crossed after pillar is collected, rotating evaporation temperature is 45 DEG C；
The sample after above-mentioned rotary evaporation is collected, ESR is put into and detects in special quartz ampoule；
Quartz ampoule is put into ESR resonators, detected, ESR central magnetic field intensity is 3500G, and microwave power is
1.86mW, microwave frequency 9.85GHz, multiplication factor are 1.00 × 106, modulation amplitude 1.00G；Modulating frequency is
100kHz；Time constant is 240ms；Sweep time is 245.76s, and its peak height value is 0.874 × 106。
Embodiment 5
Take the pork 1.5g of refrigeration 7 days；
2ml is added into meat, 150mM POBN solution is incubated, and is incubated 40min；
8ml chloroform methanols are added into above-mentioned system and mix molten, volume ratio 2:1 and 5ml deionized waters；
Above-mentioned system is homogenized；
Add 35ml chloroform methanol mixed solutions again into above-mentioned system, the two volume ratio is 2:1；
Above-mentioned system 4min is vibrated on turbula shaker；
10min is then centrifuged to above-mentioned system with 1000g centrifugal force；
Chloroform layer is separated from system with separatory funnel：
Chloroformic solution is collected after sodium peroxydisulfate pillar；
The above-mentioned chloroformic solution rotary evaporation removal chloroform crossed after pillar is collected, rotating evaporation temperature is 50 DEG C；
The sample after above-mentioned rotary evaporation is collected, ESR is put into and detects in special quartz ampoule；
Quartz ampoule is put into ESR resonators, detected, ESR central magnetic field intensity is 3500G, and microwave power is
1.86mW, microwave frequency 9.85GHz, multiplication factor are 1.00 × 106, modulation amplitude 1.00G；Modulating frequency is
100kHz；Time constant is 240ms；Sweep time is 245.76s, and its peak height value is 0.736 × 106。
Above example is only the exemplary embodiment of the present invention, is not used in the limitation present invention, protection scope of the present invention
It is defined by the claims.Those skilled in the art can make respectively in the essence and protection domain of the present invention to the present invention
Kind modification or equivalent substitution, this modification or equivalent substitution also should be regarded as being within the scope of the present invention.
Claims (8)
1. the method for lipid oxidation, comprises the following steps in a kind of quick detection meat cold storage procedure：
Step 1, the meat sample after the refrigeration of constant weight is taken；
Step 2, a- (4- pyridine radicals -1- oxygen)-N- tert-butyl group nitroketone solution that concentration is 0.1~200mM is added into sample
After be incubated；
Step 3, chloroform and methanol mixed solution and deionized water are added into step 2 system；
Step 4, step 3 system is homogenized；
Step 5, chloroform and methanol mixed solution are added into step 4 system；
Step 6, the system of oscillation step 5 on turbula shaker；
Step 7, then step 6 system is centrifuged；
Step 8, chloroform layer is separated from the system after centrifugation；
Step 9, isolated chloroformic solution is collected after sodium peroxydisulfate post；
Step 10, the chloroformic solution rotary evaporation in collection step 9 removes chloroform, and rotating evaporation temperature is 30~70 DEG C；
Step 11, the sample in collection step 10 after rotary evaporation, it is put into electron spin resonance detection quartz ampoule；
Step 12, quartz ampoule is put into electron spin resonanceapparatus and detected, wherein, the central magnetic field of electron spin resonanceapparatus
Intensity is 3500G, microwave power 1.86mW, microwave frequency 9.85GHz, and multiplication factor is 1.00 × 106, modulation amplitude is
1.00G, modulating frequency 100kHz, time constant 240ms, sweep time 245.76s.
2. the method for lipid oxidation in quick detection meat cold storage procedure according to claim 1, it is characterised in that step
In 1, the weight of meat sample is 0.5~2g.
3. the method for lipid oxidation in quick detection meat cold storage procedure according to claim 2, it is characterised in that step
In 2, the volume of a- (4- pyridine radicals -1- oxygen)-N- tert-butyl group nitroketone solution is 1~4ml；Incubation time is 10~60min, is incubated
Temperature is educated for 0 DEG C.
4. the method for lipid oxidation in quick detection meat cold storage procedure according to claim 1, it is characterised in that in step
In rapid 3, the chloroform is 1 with the volume ratio of the two in methanol mixed solution:1-5:1, chloroform methanol mixed solution cumulative volume is 1
~10ml, the addition of deionized water is 1~8ml.
5. the method for lipid oxidation in quick detection meat cold storage procedure according to claim 1, it is characterised in that in step
In rapid 5, the ratio of the two is 1 in chloroform and the methanol mixed solution:1-5:1, chloroform methanol mixed solution cumulative volume is 10
~40ml.
6. the method for lipid oxidation in quick detection meat cold storage procedure according to claim 1, it is characterised in that in step
In rapid 6, the vortex oscillation time is 2~5min.
7. the method for lipid oxidation in quick detection meat cold storage procedure according to claim 1, it is characterised in that in step
In rapid 7, centrifugal force is 500~1000g, and centrifugation time is 5~15min.
8. the method for lipid oxidation in quick detection meat cold storage procedure according to claim 1, it is characterised in that in step
In rapid 8, chloroform layer is separated from the system after centrifugation using separatory funnel.
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