CN106645446A - Fingerprint chromatogram detection method for fresh degree of abalone viscera - Google Patents
Fingerprint chromatogram detection method for fresh degree of abalone viscera Download PDFInfo
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Abstract
The invention relates to a fingerprint chromatogram detection method for fresh degree of abalone viscera. The fingerprint chromatogram detection method includes the steps: taking the abalone viscera as raw materials; cleaning the abalone viscera, and performing pulping for the cleaned abalone viscera; detecting components of the abalone viscera at corruption phases of different degrees by the aid of a headspace-solid-phase micro-extraction/gas chromatography-mass spectrometry technologies according to vacuum freezing and drying technologies; analyzing chromatogram information of the abalone viscera by the aid of a PLS-DA (partial least squares-discriminatory analysis) method to obtain results, and applying the results to fish oil extraction process of various marine products and identification of various marine products of different varieties and different production places. The method is applicable to preprocessing stages of production of various fish oil and used for improving generation quality of various fish oil, slowly solving the problem of current intense food safety and facilitating healthy and sustainable development of food health care industries, tailings of aquatic products are sufficiently used, resources cannot be wasted, and environmental protection is facilitated.
Description
Technical field
The present invention relates to aquatic products intensive processing and quality control field, more particularly to a kind of abalone internal organ freshness
Fingerprint atlas detection method.
Background technology
Fish oil is derived from the extract of abyssal fishes fat, belongs to fish tallow class.Phosphatide contained by fish oil is animal brain, god
Indispensable part in Jing tissues, marrow, the heart, liver, ovum and spleen, while contributing to digesting and assimilating, transporting and shape for fat
Into being again biomembranous important feature material.Fish oil is polyunsaturated fatty acid (DHA and EPA) rich in ω -3, can reduce people
LDL-C in body blood, reduces the viscosity of blood, with blood fat is adjusted, prevents blood clotting, prevents
The health benefits such as cerebral thrombus, cerebral hemorrhage and apoplexy, anti-inflammatory.
Abalone is nutritious, ranks one of " marine products eight delicacies ", have the good reputation of " soft gold ".China's abalone yield occupies the world
First, 2011, China's abalone culture yield reached 76786 tons, accounted for the 86% of world's cultivation total output, annual value of production more than 100 hundred million
Unit.Abalone culture increase of production is swift and violent, and 2015 annual productions are 127967 tons.In abalone process, the big of its body weight 1/3 is accounted for
Amount abalone internal organ are dropped, or are simply processed into feed, cause the very big wasting of resources and environmental pollution.These tissues
In rich in have anti-inflammatory, such as anti-oxidant, antifatigue, antitumor action lipidic biomass active component, polysaccharide, protein, amino
Acid, fat, sex hormone etc..If the high nutritive value of these products is developed, nutrition and health care, skin nursing are converted into very
To high margin products such as medicines, market potential is had much.
Meanwhile, the deterioration of abalone interior fat, such as oxidation, degraded, smell, the change of flavor components etc. are that abalone is new
The important indicator of freshness.Heavy metal or He Ermeng pollute, and significant portion is accumulated in internal organ, in various microorganisms and enzyme,
And in suitable temperature and humidity environment, internal organ easily occur corruption, its fat constituent and protein component are degraded,
Oxidation, the alkaline nitrogenous thing such as generation ammonia (NH) and amine (R-NH), thus the meeting generation bad smell after corruption, the metabolism of microorganism,
The change that Food Chemistry can be caused to constitute, and produce various corruptibility products.For example, trimethylamine has fish raw meat foul smell.Oxidation three
Methylamine is present in the internal of abalone, and balance is impregnated with for regulation when it lives, after death, in anaerobe or the work of enzyme
With under, TMAO is easy to degrade and generates the derivative of the aliphatic amines such as trimethylamine, dimethylamine, produces fishy smell;Because of insatiable hunger
It is high with content of fatty acid, it is more easy to oxidation change raw meat;Unrighted acid produces hydrogen when there is enzymatic oxidation or autoxidation
Peroxide, hydroperoxides can further decompose into many volatile small molecule aldehyde, ketone, acid etc., and these secondary oxygen
The formation for changing product is also the main cause that fishy smell is produced, and high fat content fish produce more in storage than low fat fish
Fishy smell material, and fat oxidation degree is higher, and fishy smell is denseer;After internal organ freshness changes, its local flavor occurs a series of
Change, and then have impact on the freshness and flavor components of whole abalone.
The production of China's fish oil will meet many standards, just can be promoted, particularly Fish oil, meet SC/T
In 3502-2000 outside the basic physical and chemical of fish oil, it is necessary to meet the content requirement of EPA, DHA in ST/T3503-2000.Cause
This, it is necessary to abalone internal organ freshness is rigid in checking up, the safety and Health of the fish oil of production, therefore this patent is just can ensure that
For this problem, the detection method of the freshness of its raw material abalone internal organ is probed into, it is ensured that it is most safely and effectively stored up
The Tibetan phase.
Finger-print detection refers to certain standby inspection material Jing after sample preparation process, and the analysis means for using obtain indicating
The method of the chromatogram of tested substance feature, finger-print had both had the true and false that can judge the grease essence, can reflect again
The characteristic of the different sources, Different Harvesting Time and the grease produced using various processes of oil plant of the same race such that it is able to
The quality for being detected grease is controlled on the whole.The typically conventional algorithm of grease finger-print has correlation coefficient process, included angle cosine
Method, Furthest Neighbor, what its algorithm was typically all directly quoted is the algorithm of ripe traditional Chinese medicine fingerprint.To grease finger-print algorithm
The adaptation Journal of Sex Research for carrying out independent studies, comparative study, weight distribution research and each algorithm is less.Therefore, it is necessary to existing
On some technical merits, research is related to a kind of simple operation, can it is accurately quick, comprehensively by abalone internal organ by the degree of degenerating not
Identify that abalone internal organ degenerate degree with the difference of the composition for causing.
The content of the invention
In view of this, it is an object of the invention to provide a kind of fingerprint atlas detection method of bright abalone internal organ freshness,
The research of degree is degenerated to abalone internal organ based on HS-SPME-GC-MS and PLS-DA methods and is applied in the application of preservation term, should
Method accurately, fast and efficiently differentiates to the carrying out that abalone internal organ degenerate degree.
The present invention is realized using below scheme:A kind of fingerprint atlas detection method of abalone internal organ freshness, including with
Lower step:
Step S1:Abalone internal organ are carried out to obtain abalone internal organ sample based on the process of HS-SPME;
Step S2:Gas phase and mass spectrometric parameter are configured, the GC-MS spectrograms letter of the abalone internal organ sample is gathered
Breath;
Step S3:The GC-MS spectrogram informations of the abalone internal organ sample are analyzed using PLS-DA methods, testing result is drawn.
Further, in step S1, abalone internal organ extracted successively, be enriched with, concentrated and desorbed with four process
Process, specially:The abalone internal organ of the placement different time condition for cleaning up are broken into pulpous state using homogenizer, is weighed
Certain quality, presses 2 in ml headspace bottle:7-4:7 solid-liquid ratio adds saturated nacl aqueous solution, pre- under certain preheating temperature T
Hot a period of time t, promotes SPME handles extracting fiber head to be stretched into ml headspace bottle, in being subsequently placed in magnetic agitation heater,
Stable equilibrium temperature T1Under, regular hour t is kept under certain rotating speed R1, extracting fiber head is withdrawn, take out from ml headspace bottle
SPME handles, and be inserted into the injection port of GC-MS, parse a period of time t in gas chromatographic sample introduction mouth2。
Further, it is built-in with magnetic rotor in the ml headspace bottle.
Further, in step S3, the GC-MS spectrogram informations of abalone internal organ sample are analyzed using PLS-DA methods, is obtained
Go out result, specifically include following steps:
Step S3-1:Establishing criteria mass spectrum picture library to the GC-MS collection of illustrative plates of the abalone internal organ sample of different corruption degree into
Divide to enter line retrieval qualitative, quantitative analysis is carried out using area normalization method, extract the total information of sample component, use total chemical
The peak area of composition is index, and the abalone internal organ sample with different corruption degree builds becoming certainly for training sample as class
Moment matrix X, and set classified variable matrix Y;
Step S3-2:The independent variable matrix X and classified variable matrix Y of training sample are decomposed with PLS homing methods,
And the maximum linear correlation of principal component of X and Y is caused, its model is expressed as:
X=TPT+E
Y=UQT+F
Wherein, T and U are respectively the score matrix of X and Y, and P and Q is respectively the loading matrix of X and Y, and E and F is respectively X and Y
Residual matrix, subscript T represents transposition computing;
Step S3-3:T and U are made into linear regression:U=TB, during prediction sample to be tested, according to P obtaining for sample to be tested x is obtained
Point vector t, finally tries to achieve predicted value y=tBQ, and the classification according to the value of y to sample to be tested judges, wherein, regression vectors B
=(TTT)-1TTU。
Further, the extracting fiber head adopts 50/30 μm of DVB/CAR/PDMS fiber heads, and the extracting fiber
The head aging 1h under conditions of 250 DEG C of injector temperature before the use.
Further, preheating temperature T is 25-35 DEG C, equilibrium temperature T1For 65-80 DEG C, rotating speed R is 75-100rad/
Min, time t are 10-20min, t1For 40-60min, t2For 5min.
Further, in step S2, during collection abalone internal organ sample GC-MS spectrogram informations, chromatographic condition includes:
The DB-WAX quartz capillary columns of 30m × 0.25mm × 0.25 μm;Heating schedule is first to keep 2min with 35 DEG C of temperature, then with 5
DEG C/min rises to 120 DEG C, keeps 2min, continues to rise to 150 DEG C with 10 DEG C/min, keeps 2min, finally risen to 20 DEG C/min
240 DEG C, keep 3min;The flow velocity of He carrier gas is 1-1.2mL/min;Split ratio is 1:10–40.
Further, in step S2, during collection abalone internal organ sample GC-MS spectrogram informations, Mass Spectrometry Conditions include:EI
Ion gun;Collision cell energy is set to 40~80eV;Transmission line temperature is 200~250 DEG C;Ion source temperature is 200 DEG C;Quality is swept
Scope is retouched for 35~500.
Compared with prior art, the present invention directly applies to grease fingerprint pattern technology in fish oil production process, and has
There is detection speed fast, favorable repeatability, sensitivity is high, simple operation and other advantages, has great significance to the production safety of fish oil.
Because of the difference of storage conditions, its composition has very big difference to abalone internal organ, and the present invention is combined into by gas chromatographic analysis means
Content is divided to study with fingerprint pattern technology, can tell effectively carry out discriminatory analysis to the abalone internal organ of different corruption degree,
And fully apply to it in preservation.
Description of the drawings
Fig. 1 is method of the present invention schematic flow sheet.
Fig. 2 is that 0h detections obtain GC-MS spectrograms in the embodiment of the present invention.
Fig. 3 is that 12h detections obtain GC-MS spectrograms in the embodiment of the present invention.
Fig. 4 is that 24h detections obtain GC-MS spectrograms in the embodiment of the present invention.
Fig. 5 is that 48h detections obtain GC-MS spectrograms in the embodiment of the present invention.
Specific embodiment
Below in conjunction with the accompanying drawings and embodiment the present invention will be further described.
This enforcement adopts two groups of control groups, respectively organizes one:Normal temperature (25 DEG C) group, group two:Refrigeration (4 DEG C) group.Wherein, often
Temperature group includes eight samples:0h, 3h, 6h, 12h, 24h, 36h, 48h, 72h;Refrigeration group is corresponding.
As shown in figure 1, step 1:Group one, two samples of group are carried out respectively based on the pre-treatment of HS-SPME.
Take group one, two samples of group each 10 groups, beat into slurry, respectively take 0.3g or so in 4mL ml headspace bottles, add certain volume
Saturated aqueous common salt (m:V=2:7–4:7), 10-20min are preheated in 25-35 DEG C, pushes away SPME handles and stretch into extracting head fiber head
In ml headspace bottle, be subsequently placed in equilibrium temperature be 65-80 DEG C of rotating speeds be on the magnetic agitation heater of 75-100rad/min, to keep
Extracting fiber head is withdrawn after 40-60min, solid phase handle is taken out, the injection port of GC-MS is inserted into, in gas chromatographic sample introduction mouth solution
Inhale 5min.
Step 2:The GC-MS spectrogram informations collection of group one, two samples of group is carried out respectively.
Gas phase and mass spectrometric parameter are set, and design parameter is as follows:
Chromatographic condition:(1) the DB-WAX quartz capillary columns of 30m × 0.25mm × 0.25 μm;(2) heating schedule:First with 35
DEG C temperature keep 2min, then rise to 120 DEG C with 5 DEG C/min, keep 2min, continue to rise to 150 DEG C with 10 DEG C/min, keep
2min, finally rises to 240 DEG C with 20 DEG C/min, keeps 3min;(3) flow velocity of He carrier gas is 1-1.2mL/min;(4) split ratio:
1:10–40。
Mass Spectrometry Conditions:EI ion guns;Electron energy is set to 40~80eV;200~250 DEG C of transmission line temperature;Ion gun temperature
200 DEG C of degree;Mass scan range is between 35~500.
After instrument stabilizer, 160 samples obtained through processing pre-treatment in step 1 are carried out into auto injection analysis.
Step 3:The GC-MS spectrogram informations of all samples are analyzed using PLS-DA methods, are obtained a result, including it is following
Step:
(1) retrieval is carried out to the composition foundation NIST and standard mass spectrum picture library of GC-MS collection of illustrative plates qualitative, using area normalization
Method carries out quantitative analysis.The total information of 160 sample components is extracted, the peak area with total chemical composition is index, with 16
160 samples of group are class, build the independent variable matrix X of training sample, and set classified variable matrix Y, due to
The sample that this example is implemented is from two class degree, therefore matrix Y is bivector.
(2) the independent variable matrix X and classified variable matrix Y of training sample are decomposed with PLS homing methods, and is made
The maximum linear correlation of principal component of X and Y is obtained, its model is expressed as:
X=TPT+E
Y=UQT+F
Wherein, T and U are respectively the score matrix of X and Y, and P and Q is respectively the loading matrix of X and Y, and E and F is respectively X and Y
Residual matrix;
(3) T and U are made into linear regression:U=TB, during prediction sample to be tested, according to P the score vector of sample to be tested x is obtained
T, finally tries to achieve predicted value y=tBQ, and the classification according to the value of y to sample to be tested judges, wherein, regression vectors B=
(TTT)-1TTU。
For the category classification problem of n class samples, using n-1 PLS-DA sub-classifiers series connection complete dividing is realized
Class.Basic ideas are, the 1st grader separates in the 1st class and 2,3...n class sample, the 2nd grader by the 2nd classification and
3,4...n classifications separate, by that analogy, until all of classification is separated.In the present embodiment, it is necessary to using 1
PLS-DA sub-classifiers connect to realize classification.
Embodiment 1
A kind of fingerprint atlas detection method of abalone internal organ freshness, comprise the following steps (carries out 10 groups to enter with batch
Row processing detection):
(1) abalone internal organ sample is carried out based on the pre-treatment of HS-SPME:The fresh abalone bought back is carried out except internal organ,
Internal organ are carried out into homogenate weighing, every 0.3g or so is portion in valve bag, is blown into nitrogen, and nominal takes 15 samples, and No. 1 is first carried out
The detection of 0h, remaining per 7 be one group, be divided into two groups, carry out the storage of different groups, respectively at 4 DEG C refrigeration, another group in
25 DEG C of insulating boxs.First carry out the detection of 0h:Weigh 0.3217g internal organ to be homogenized in 4mL ml headspace bottles, add the saturation food of 1.4mL
Salt solution, in 30 DEG C 10min is preheated, and is pushed away SPME handles and extracting head fiber head is stretched into ml headspace bottle, and being subsequently placed in equilibrium temperature is
80 DEG C of rotating speeds take out solid phase handle on the magnetic agitation heater of 90rad/min, to keep withdrawing extracting fiber head after 40min,
The injection port of GC-MS is inserted into, in gas chromatographic sample introduction mouth 5min is desorbed.
(2) the GC-MS spectrogram informations collection of group one, two samples of group is carried out respectively.
Gas phase and mass spectrometric parameter are set, and design parameter is as follows:
Chromatographic condition:(1) the DB-WAX quartz capillary columns of 30m × 0.25mm × 0.25 μm;(2) heating schedule:First with 35
DEG C temperature keep 2min, then rise to 120 DEG C with 5 DEG C/min, keep 2min, continue to rise to 150 DEG C with 10 DEG C/min, keep
2min, finally rises to 240 DEG C with 20 DEG C/min, keeps 3min;(3) flow velocity of He carrier gas is 1mL/min;(4) split ratio:1:
10。
Mass Spectrometry Conditions:EI ion guns;Electron energy is set to 70eV;230 DEG C of transmission line temperature;200 DEG C of ion source temperature;Matter
Amount sweep limits is between 35~500.
(3) the GC-MS spectrogram informations of all samples are analyzed using PLS-DA methods, are obtained a result.
Embodiment 2
A kind of fingerprint atlas detection method of abalone internal organ freshness, comprise the following steps (carries out 10 groups to enter with batch
Row processing detection):
(1) abalone internal organ sample is carried out based on the pre-treatment of HS-SPME:The fresh abalone bought back is carried out except internal organ,
Internal organ are carried out into homogenate weighing, every 0.3g or so is portion in valve bag, is blown into nitrogen, and nominal takes 15 samples, and No. 1 is first carried out
The detection of 0h, remaining per 7 be one group, be divided into two groups, carry out the storage of different groups, respectively at 4 DEG C refrigeration, another group in
25 DEG C of insulating boxs.First carry out the detection of 0h:Weigh 0.4112g internal organ to be homogenized in 4mL ml headspace bottles, add the saturation food of 1.5mL
Salt solution, in 35 DEG C 15min is preheated, and is pushed away SPME handles and extracting head fiber head is stretched into ml headspace bottle, and being subsequently placed in equilibrium temperature is
70 DEG C of rotating speeds take out solid phase handle on the magnetic agitation heater of 85rad/min, to keep withdrawing extracting fiber head after 60min,
The injection port of GC-MS is inserted into, in gas chromatographic sample introduction mouth 5min is desorbed.
(2) the GC-MS spectrogram informations collection of group one, two samples of group is carried out respectively, and gas phase and mass spectrometric parameter, tool are set
Body parameter is as follows:
Chromatographic condition:(1) the DB-WAX quartz capillary columns of 30m × 0.25mm × 0.25 μm;(2) heating schedule:First with 35
DEG C temperature keep 2min, then rise to 120 DEG C with 5 DEG C/min, keep 2min, continue to rise to 150 DEG C with 10 DEG C/min, keep
2min, finally rises to 240 DEG C with 20 DEG C/min, keeps 3min;(3) flow velocity of He carrier gas is 1mL/min;(4) split ratio:1:
40。
Mass Spectrometry Conditions:EI ion guns;Electron energy is set to 70eV;230 DEG C of transmission line temperature;200 DEG C of ion source temperature;Matter
Amount sweep limits is between 35~500.
Normal temperature group such as Fig. 2,3,4,5, wherein, refrigeration group composition in 3 days changes not substantially, therefore with the collection of illustrative plates of normal temperature group
As optimal case.
(3) the GC-MS spectrogram informations of all samples are analyzed using PLS-DA methods:Establishing criteria mass spectrum picture library
(NIST) line retrieval is entered to the composition of the GC-MS collection of illustrative plates of the abalone internal organ sample of different corruption degree qualitative, using area normalization
Change method carries out quantitative analysis, extracts the total information of sample component, and the peak area with total chemical composition is index, by Fig. 2,3,
4th, 5 understand, by the change of wherein significant composition, such as, as storage phase changes, the alkalescence such as ammonia (NH) and amine (R-NH) contains
The peak height and area of nitrogen thing such as dramatically increases at the change, and some flavor components alcohol, ketone, naphthalenes etc. are substantially reduced, and are utilized
Its result be inferred by PLS-DA methods, judged its freshness.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent with
Modification, should all belong to the covering scope of the present invention.
Claims (8)
1. a kind of fingerprint atlas detection method of abalone internal organ freshness, it is characterised in that:Comprise the following steps:
Step S1:Abalone internal organ are carried out to obtain abalone internal organ sample based on the process of HS-SPME;
Step S2:Gas phase and mass spectrometric parameter are configured, the GC-MS spectrogram informations of the abalone internal organ sample are gathered;
Step S3:The GC-MS spectrogram informations of the abalone internal organ sample are analyzed using PLS-DA methods, testing result is drawn.
2. the fingerprint atlas detection method of a kind of abalone internal organ freshness according to claim 1, it is characterised in that:Institute
In stating step S1, abalone internal organ extracted successively, be enriched with, concentrated and desorbed with four processing procedures, specially:Cleaning is dry
The abalone internal organ of net placement different time condition break into pulpous state using homogenizer, certain quality are weighed, in ml headspace bottle
In press 2:7-4:7 solid-liquid ratio adds saturated nacl aqueous solution, the preheated one-section time t under certain preheating temperature T to promote SPME
Handle stretches into extracting fiber head in ml headspace bottle, in being subsequently placed in magnetic agitation heater, in stable equilibrium temperature T1Under, one
Determine to keep regular hour t under rotating speed R1, extracting fiber head is withdrawn, SPME handles are taken out from ml headspace bottle, and it is inserted into GC-MS
Injection port in, parse a period of time t in gas chromatographic sample introduction mouth2。
3. the fingerprint atlas detection method of a kind of abalone internal organ freshness according to claim 2, it is characterised in that:Institute
State and be built-in with ml headspace bottle magnetic rotor.
4. the fingerprint atlas detection method of a kind of abalone internal organ freshness according to claim 1, it is characterised in that:Institute
In stating step S3, the GC-MS spectrogram informations of abalone internal organ sample are analyzed using PLS-DA methods, obtained a result, specifically included following
Step:
Step S3-1:Establishing criteria mass spectrum picture library enters to the composition of the GC-MS collection of illustrative plates of the abalone internal organ sample of different corruption degree
Line retrieval is qualitative, and using area normalization method quantitative analysis is carried out, and extracts the total information of sample component, uses total chemical composition
Peak area be index, the abalone internal organ sample with different corruption degree as class, build training sample independent variable square
Battle array X, and set classified variable matrix Y;
Step S3-2:The independent variable matrix X and classified variable matrix Y of training sample are decomposed with PLS homing methods, and is made
The maximum linear correlation of principal component of X and Y is obtained, its model is expressed as:
X=TPT+E
Y=UQT+F
Wherein, T and U are respectively the score matrix of X and Y, and P and Q is respectively the loading matrix of X and Y, and E and F is respectively the residual of X and Y
Difference matrix, subscript T represents transposition computing;
Step S3-3:T and U are made into linear regression:U=TB, during prediction sample to be tested, according to P obtain the score of sample to be tested x to
Amount t, finally tries to achieve predicted value y=tBQ, and the classification according to the value of y to sample to be tested judges, wherein, regression vectors B=
(TTT)-1TTU。
5. the fingerprint atlas detection method of a kind of abalone internal organ freshness according to claim 2, it is characterised in that:Institute
The DVB/CAR/PDMS fiber heads that extracting fiber head is using 50/30 μm are stated, and the extracting fiber head is before the use in sample introduction
Aging 1h under conditions of 250 DEG C of temperature of mouth.
6. the fingerprint atlas detection method of a kind of abalone internal organ freshness according to claim 2, it is characterised in that:Institute
It is 25-35 DEG C to state preheating temperature T, equilibrium temperature T1For 65-80 DEG C, rotating speed R is 75-100rad/min, time t is 10-
20min, t1For 40-60min, t2For 5min.
7. the fingerprint atlas detection method of a kind of abalone internal organ freshness according to claim 1, it is characterised in that:Institute
In stating step S2, during collection abalone internal organ sample GC-MS spectrogram informations, chromatographic condition includes:30m × 0.25mm × 0.25 μm
DB-WAX quartz capillary columns;Heating schedule is first to keep 2min with 35 DEG C of temperature, then rises to 120 DEG C with 5 DEG C/min, is kept
2min, continues to rise to 150 DEG C with 10 DEG C/min, keeps 2min, finally rises to 240 DEG C with 20 DEG C/min, keeps 3min;He carrier gas
Flow velocity be 1-1.2mL/min;Split ratio is 1:10–40.
8. the fingerprint atlas detection method of a kind of abalone internal organ freshness according to claim 1, it is characterised in that:Institute
In stating step S2, during collection abalone internal organ sample GC-MS spectrogram informations, Mass Spectrometry Conditions include:EI ion guns;Collision cell energy sets
For 40~80eV;Transmission line temperature is 200~250 DEG C;Ion source temperature is 200 DEG C;Mass scan range is 35~500.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107389823A (en) * | 2017-07-31 | 2017-11-24 | 江苏省环境监测中心 | The method of SPME analysis of off-flavors system detectio pickles factory uncontrollable discharge smell substance |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104764831A (en) * | 2015-04-27 | 2015-07-08 | 江苏易谱恒科技有限公司 | Cake essence and flavor identifying method based on HS-SPME-GC-MS and PLS-DA methods |
CN105628883A (en) * | 2015-12-31 | 2016-06-01 | 浙江海洋学院 | Ethyl ester type fish oil quality evaluation method based on electronic nose analysis |
-
2016
- 2016-09-28 CN CN201610858244.2A patent/CN106645446B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104764831A (en) * | 2015-04-27 | 2015-07-08 | 江苏易谱恒科技有限公司 | Cake essence and flavor identifying method based on HS-SPME-GC-MS and PLS-DA methods |
CN105628883A (en) * | 2015-12-31 | 2016-06-01 | 浙江海洋学院 | Ethyl ester type fish oil quality evaluation method based on electronic nose analysis |
Non-Patent Citations (3)
Title |
---|
HONG-XU WANG等: "Effects of heating conditions on fatty acids and volatile compounds in foot muscle of abalone Haliotis discus hannai Ino", 《FOOD SCIENCE AND TECHNOLOGY》 * |
李阳等: "武昌鱼中挥发性成分的HS-SPME和GC-MS分析", 《湖北农业科学》 * |
郑瑞生等: "固相微萃取与气-质联用法分析鲍鱼烘烤前后挥发性成分的变化", 《现代食品科技》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107389823A (en) * | 2017-07-31 | 2017-11-24 | 江苏省环境监测中心 | The method of SPME analysis of off-flavors system detectio pickles factory uncontrollable discharge smell substance |
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