CN106645484B - The identification method of dried meat floss product of poor quality - Google Patents
The identification method of dried meat floss product of poor quality Download PDFInfo
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- 241000628997 Flos Species 0.000 title claims abstract description 50
- 235000015177 dried meat Nutrition 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000049 pigment Substances 0.000 claims abstract description 25
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims abstract description 15
- 239000003960 organic solvent Substances 0.000 claims abstract description 11
- 239000000470 constituent Substances 0.000 claims abstract description 5
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 48
- 239000006193 liquid solution Substances 0.000 claims description 47
- 239000000243 solution Substances 0.000 claims description 39
- 239000007788 liquid Substances 0.000 claims description 28
- 239000007864 aqueous solution Substances 0.000 claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 239000004952 Polyamide Substances 0.000 claims description 14
- 229920002647 polyamide Polymers 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 12
- 238000012546 transfer Methods 0.000 claims description 12
- 239000000284 extract Substances 0.000 claims description 11
- 239000004615 ingredient Substances 0.000 claims description 11
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 10
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 10
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 239000007790 solid phase Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 7
- 239000003208 petroleum Substances 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 5
- 239000005695 Ammonium acetate Substances 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000019257 ammonium acetate Nutrition 0.000 claims description 5
- 229940043376 ammonium acetate Drugs 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- 239000007791 liquid phase Substances 0.000 claims description 5
- 239000012071 phase Substances 0.000 claims description 5
- 238000002390 rotary evaporation Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 238000004587 chromatography analysis Methods 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 239000000975 dye Substances 0.000 claims description 4
- 230000014759 maintenance of location Effects 0.000 claims description 4
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 238000010025 steaming Methods 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 238000010812 external standard method Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000005374 membrane filtration Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 235000013399 edible fruits Nutrition 0.000 claims 1
- 150000002825 nitriles Chemical class 0.000 claims 1
- 238000009210 therapy by ultrasound Methods 0.000 claims 1
- 210000004885 white matter Anatomy 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 16
- 235000005979 Citrus limon Nutrition 0.000 abstract description 10
- 102000004169 proteins and genes Human genes 0.000 abstract description 8
- 108090000623 proteins and genes Proteins 0.000 abstract description 8
- 238000011084 recovery Methods 0.000 abstract description 7
- 241000220317 Rosa Species 0.000 abstract description 6
- 239000012488 sample solution Substances 0.000 abstract description 5
- 150000004676 glycans Chemical class 0.000 abstract description 3
- 229920001282 polysaccharide Polymers 0.000 abstract description 3
- 239000005017 polysaccharide Substances 0.000 abstract description 3
- 230000001112 coagulating effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 244000248349 Citrus limon Species 0.000 abstract 1
- 239000000047 product Substances 0.000 description 12
- 244000131522 Citrus pyriformis Species 0.000 description 9
- 239000000523 sample Substances 0.000 description 8
- 239000012086 standard solution Substances 0.000 description 7
- 235000018102 proteins Nutrition 0.000 description 6
- 235000012730 carminic acid Nutrition 0.000 description 4
- 230000001419 dependent effect Effects 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 235000019764 Soybean Meal Nutrition 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000003086 colorant Substances 0.000 description 3
- 239000004455 soybean meal Substances 0.000 description 3
- 239000011550 stock solution Substances 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 235000020997 lean meat Nutrition 0.000 description 2
- 244000144977 poultry Species 0.000 description 2
- 235000004252 protein component Nutrition 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- CAXNYFPECZCGFK-UHFFFAOYSA-N 2-phenyl-2-pyridin-2-ylacetonitrile Chemical compound C=1C=CC=NC=1C(C#N)C1=CC=CC=C1 CAXNYFPECZCGFK-UHFFFAOYSA-N 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- SVWLIIFHXFGESG-UHFFFAOYSA-N formic acid;methanol Chemical compound OC.OC=O SVWLIIFHXFGESG-UHFFFAOYSA-N 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 235000013622 meat product Nutrition 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- GOLXNESZZPUPJE-UHFFFAOYSA-N spiromesifen Chemical compound CC1=CC(C)=CC(C)=C1C(C(O1)=O)=C(OC(=O)CC(C)(C)C)C11CCCC1 GOLXNESZZPUPJE-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Landscapes
- Physics & Mathematics (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)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The present invention relates to a kind of identification methods of dried meat floss product of poor quality.Whether the identification method of the dried meat floss of poor quality is adulterated to identify dried meat floss by the method for pigment in detection dried meat floss, the synthetic dyestuffs such as sunset yellow, lemon yellow, famille rose, the Wang Jinhuang in dried meat floss can be detected simultaneously, it is whether adulterated to identify dried meat floss by having no added pigment in detection dried meat floss.The identification method is readily soluble in water using pigment, the minimum characteristic of solubility removes fat constituent first in most of organic solvent, make protein coagulative precipitation using the method saltoutd and goes the interference of isolating protein, using the interference of solid phase extraction Polysaccharide removing and natural pigment, and concentrating sample solution.The identification method solves the problems, such as that the Wang Jinhuang Solid Phase Extraction rate of recovery is low, and good separating effect, specificity is strong, and detection limit and quantitative limit are sufficiently low, and the range of linearity is good, reproducible, accurately and reliably, can be used for day-to-day supervision detection.
Description
Technical field
The present invention relates to field of food detection, more particularly, to a kind of identification method of dried meat floss product of poor quality.
Background technique
Dried meat floss refers to that with fowl, poultry lean meat be primary raw material, and cooked, stripping and slicing, ingredient, receives soup, stir-fry is loose, rubs pine with the hands etc. at oil skimming
Fiber fluffy made of step is at cotton-shaped meat products.90% or more ingredient is by moisture, protein, fat, more in dried meat floss
Sugar is constituted, wherein the content of protein is generally between 30%~60%.
In recent years, the demand usage amount with dried meat floss is increasing, various dried meat floss products of poor quality are also mixed into market therewith.
The soybean meal for having squeezed oil just contains the protein and polysaccharide of very high-content, content in dried meat floss protein and polyoses content connect
Closely, so often occurring pretending to be dried meat floss by processing using soybean meal as the soyabean protein powder of raw material in the market.These illegal rows
To not only break up fair trading, loss is brought to consumer and the real dried meat floss producer, and since soybean meal is at
Reason is formed by " dried meat floss " and distinguishes with fowl, poultry lean meat dried meat floss obviously, so it is generally necessary to being dyed with colorant in color.
The coloring agent being commonly used has the synthetic dyestuffs such as lemon yellow, sunset yellow, Wang Jinhuang, famille rose.In mandatory national standards " GB
2760-2014 national food safety standard food additives use standard " in, these pigments all forbid addition, long-term to eat
With synthetic dyestuff, allergy can be easy to cause, even liver and kidney are damaged.
Currently, the method that people mainly use sense organ to judge identifies the true and false of dried meat floss, including pinched with hand, eyes are seen, mouth
The mode of trial test identifies dried meat floss, but requirement of this method for identification person is so high, identification result accuracy and reliability
It is not high.
Summary of the invention
Based on this, it is necessary to for the not high problem of the accuracy and reliability of traditional dried meat floss product testing, provide
A kind of identification method of dried meat floss product of poor quality.
The technical solution that the present invention solves above-mentioned technical problem is as follows.
A kind of identification method of dried meat floss product of poor quality, includes the following steps:
Step 1: organic solvent is added into the sample of dried meat floss product and extracts fat constituent therein, volatilizes described organic
Solvent collects solid phase；
Step 2: being added acetonitrile solution into the solid phase that step 1 obtains, and extracts pigment composition therein, is centrifuged, and receives
Collect liquid solution；
Step 3: ammonium sulfate will be added after the liquid solution concentration of step 2 collection, wherein with precipitating removal
Protein component, centrifugation, collect liquid solution；
Step 4: after the liquid solution that step 3 is collected is blown to net do, it is transferred to polyamide solid phase extraction cartridge, to remove it
In natural pigment ingredient, collect liquid solution；
Step 5: the liquid solution collected in step 4 is blown to it is net dry, with water transfer it is fixed it is molten after cross high performance liquid chromatography
Instrument detects synthetic dyestuff content therein using diode array detector, and qualitative with retention time, quantified by external standard method obtains
Qualification result.
In one of the embodiments, in said step 1, organic solvent used be initial boiling point not less than 30 DEG C and
The end point of distillation is not higher than 60 DEG C of petroleum ether.
In one of the embodiments, in the step 2, the volumetric concentration of the acetonitrile solution is 70%；
The extraction pigment composition therein is will to be added to have the solution of the acetonitrile solution to be ultrasonically treated, so as to contain
There is pigment composition to be dissolved in the acetonitrile solution, then be centrifuged, and is repeated to extract repeatedly with the acetonitrile solution until centrifugation
Extracting liquid colourless afterwards, combined extract obtain liquid solution.
In one of the embodiments, in the step 3, the liquid solution concentration that step 2 is collected
It includes: mass concentration to be added while hot as 10% institute for after liquid solution heating rotary evaporation concentration that ammonium sulfate is added afterwards
State ammonium sulfate.
In one of the embodiments, in the step 3, further includes: the precipitating being centrifuged using water washing, then
Liquid solution is collected by centrifugation, and merges each centrifugate and obtains liquid solution.
In one of the embodiments, in the step 4, the liquid solution that step 3 is collected is blown to net dry
It is that the liquid solution is blown to net do using nitrogen；
It is described to be transferred to polyamide solid phase extraction cartridge, to remove natural pigment ingredient therein, collect liquid solution include: by
It is blown to after only dry solution is transferred to polyamide solid phase extraction cartridge, first washs the polyamide using the aqueous solution of 60 DEG C of pH 4.0
Solid-phase extraction column is multiple, then uses dehydrated alcohol-ammonium hydroxide-aqueous solution to wash colourless to stripping liquid, merges each stripping liquid and obtain
Liquid solution.
The aqueous solution of the pH 4.0 is the water that ultrapure water to pH 4.0 is adjusted with citric acid in one of the embodiments,
Solution；
The volume ratio of dehydrated alcohol, ammonium hydroxide and water is 7:2:1 in the dehydrated alcohol-ammonium hydroxide-aqueous solution.
In one of the embodiments, in the step 5, the liquid solution that will be collected in step 4 is blown to only
It is dry, with water transfer it is fixed it is molten after cross high performance liquid chromatograph include: liquid solution that will be collected in step 4 with second acid for adjusting pH extremely
7.0, blow steaming to net dry using nitrogen, with water transfer it is fixed it is molten after cross high performance liquid chromatograph.
In one of the embodiments, in the step 5, further include by water transfer it is fixed it is molten after obtained solution mistake
The step of 0.22 μm of membrane filtration, test liquid of the solution obtained after filtering as the excessively described high performance liquid chromatograph.
In one of the embodiments, in the step 5, the condition of chromatography is:
Chromatographic column: the octadecylsilane chemically bonded silica column having a size of 5 μm of * 4.6mm*250mm；
Mobile phase: the mixed liquor for the ammonium acetate solution that the methanol and concentration that volume ratio is 15:85 are 20mmol/L；
Flow velocity: 1mL/min；
Column temperature: 40 DEG C；
Diode array detector wavelength used when detecting is 450nm.
Whether the identification method of above-mentioned dried meat floss of poor quality identifies dried meat floss by the method for colorant (pigment) in detection dried meat floss
It is adulterated, the synthetic dyestuffs such as sunset yellow, lemon yellow, famille rose, the Wang Jinhuang in dried meat floss can be detected simultaneously, by having in detection dried meat floss
No added pigment, it is whether adulterated to identify dried meat floss.The identification method is readily soluble in water using pigment, in most of organic solvent
The minimum characteristic of solubility removes fat constituent first, makes protein coagulative precipitation using the method saltoutd and removes isolating protein
Interference, using the interference of solid phase extraction Polysaccharide removing and natural pigment, and concentrating sample solution.The identification method solves king
The low problem of the golden yellow Solid Phase Extraction rate of recovery, good separating effect, specificity is strong, and detection limit and quantitative limit are sufficiently low, the range of linearity
Well, reproducible, accurately and reliably, it can be used for day-to-day supervision detection.
Detailed description of the invention
Fig. 1 is standard solution map, is followed successively by lemon yellow, famille rose, sunset yellow and Wang Jinhuang；
Fig. 2 is sample solution map.
Specific embodiment
To facilitate the understanding of the present invention, below in conjunction with attached drawing to invention is more fully described.But it is of the invention
It can realize in many different forms, however it is not limited to embodiment described herein.On the contrary, providing these embodiments
Purpose is to make the disclosure of the present invention more thorough and comprehensive.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
Any and all combinations of the listed item of pass.
The identification method of the dried meat floss product of poor quality of one embodiment, includes the following steps:
Step 1: being added organic solvent into the sample of dried meat floss product and extract fat constituent therein, volatilize organic solvent,
Collect solid phase.
Organic solvent used is initial boiling point not less than 30 DEG C and the end point of distillation is not higher than 60 DEG C of petroleum ether.
Step 2: being added acetonitrile solution into the solid phase that step 1 obtains, and extracts pigment composition therein, is centrifuged, and receives
Collect liquid solution.
The volumetric concentration of acetonitrile solution is preferably 70%.
Specifically extracting pigment composition therein is that will be added to have the solution of acetonitrile solution to be ultrasonically treated, such as ultrasound
10min so as to be dissolved in acetonitrile solution containing pigment composition, then is centrifuged, and is such as centrifuged 5min with 10000r/min, and use acetonitrile
Aqueous solution repeats to extract repeatedly the extracting liquid colourless after centrifugation, combined extract and obtains liquid solution.
Step 3: ammonium sulfate will be added after the liquid solution concentration of step 2 collection, wherein with precipitating removal
Protein component, centrifugation, collect liquid solution.
Specifically, liquid solution can be heated to rotary evaporation concentration, partial solvent such as is removed in 60 DEG C of rotary evaporations, then
The ammonium sulfate that mass concentration is 10% is added while hot.
Preferably, step 3 further includes the precipitating being centrifuged using water washing, then liquid solution is collected by centrifugation, and is merged
Each centrifugate obtains liquid solution.
Step 4: after the liquid solution that step 3 is collected is blown to net do, it is transferred to polyamide solid phase extraction cartridge, to remove it
In natural pigment ingredient, collect liquid solution.
It is to be blown to the liquid solution using nitrogen to do only that the liquid solution that step 3 is collected, which is blown to only dry, to remove
Remove extra organic principle, concentrating sample.
It is described to be transferred to polyamide solid phase extraction cartridge, to remove natural pigment ingredient therein, collect liquid solution include: by
It is blown to after only dry solution is transferred to polyamide solid phase extraction cartridge, first washs polyamide solid phase using the aqueous solution of 60 DEG C of pH 4.0
Extraction column is multiple, then uses dehydrated alcohol-ammonium hydroxide-aqueous solution to wash colourless to stripping liquid, merges each stripping liquid and obtain liquid phase
Solution.Preferably, the aqueous solution of pH 4.0 is the aqueous solution that ultrapure water to pH 4.0 is adjusted with citric acid；Dehydrated alcohol-ammonium hydroxide-
The volume ratio of dehydrated alcohol, ammonium hydroxide and water is 7:2:1 in aqueous solution.
Step 5: the liquid solution collected in step 4 is blown to it is net dry, with water transfer it is fixed it is molten after cross high performance liquid chromatography
Instrument detects synthetic dyestuff content therein using diode array detector, and qualitative with retention time, quantified by external standard method obtains
Qualification result.
The liquid solution that will be collected in step 4 be blown to it is net dry, with water transfer it is fixed it is molten after cross high performance liquid chromatograph packet
It includes: by the liquid solution collected in step 4 second acid for adjusting pH to 7.0, blowing steaming using nitrogen and done to net, remove ammonium hydroxide and ethyl alcohol,
Molten rear high performance liquid chromatograph excessively calmly is shifted with water.
Preferably, in step 5, further include by water transfer it is fixed it is molten after obtained solution cross 0.22 μm of membrane filtration
Step, the solution obtained after filtering were used as the test liquid of high performance liquid chromatograph.
The condition of chromatography is preferably but not limited to:
Chromatographic column: the octadecylsilane chemically bonded silica column having a size of 5 μm of * 4.6mm*250mm.
Mobile phase: the mixed liquor for the ammonium acetate solution that the methanol and concentration that volume ratio is 15:85 are 20mmol/L.
Flow velocity: 1mL/min.
Column temperature: 40 DEG C.
Diode array detector wavelength used when detecting is preferably but not limited to as 450nm.
The following are specific embodiment parts.
1. instrument and reagent
1.1 high performance liquid chromatographs (carry diode array detector).
1.2 standard substances: sunset yellow, lemon yellow, Wang Jinhuang, famille rose.
1.3 analytical reagents: ammonium acetate, ammonium sulfate, petroleum ether (30~60 DEG C), ethyl alcohol, formic acid, acetic acid, citric acid.
1.4 chromatography pure reagents: methanol, acetonitrile.
1.5 polyamide solid phases extract pillar.
The water of 1.6pH=4 adjusts ultrapure water to pH=4 with citric acid.
1.7 methanol formic acid mixed liquors: methanol: formic acid=6:4 (volume ratio).
1.8 dehydrated alcohols-ammonium hydroxide-aqueous solution: dehydrated alcohol: ammonium hydroxide: water=7:2:1 (volume ratio).
2. the preparation of standard solution
Polychrom mixes stock solution: weighing that standard substance is appropriate, and being dissolved with water and being diluted to concentration is about 1mg/mL's
Stock solution.
Polychrom standard solution: stock solution is taken to be diluted with water to the standard solution of about 50 μ g/mL of concentration.
3. sample detection
3.1 take dried meat floss product sample about 10g, set in 100mL erlenmeyer flask, add petroleum ether 50mL, and stirring discards petroleum ether,
In triplicate, volatilize, be added 70% acetonitrile solution ultrasonic extraction 10min, 10000r/min is centrifuged 5min, extracting solution be transferred to from
Heart flask repeats extraction process to extracting liquid colourless.
10% ammonium sulfate solution of 1mL is added in 60 DEG C of rotary evaporations to 5mL in 3.2 combined extracts while hot,
10000r/min is centrifuged 5min, and supernatant is transferred to new centrifuge tube, is precipitated with a little water washing, and centrifugation merges centrifugate.
Centrifugate is blown to net do using nitrogen by 3.3.
Above-mentioned solution is transferred to polyamide solid phase extraction cartridge by 3.4, is first washed 3 times using the aqueous solution of 60 DEG C of pH 4.0,
Then it is washed using dehydrated alcohol-ammonium hydroxide-aqueous solution colourless to stripping liquid.
3.5 merge stripping liquid, and using second acid for adjusting pH to 7.0, nitrogen blows steaming to be done to net, are settled to 20mL, mistake with water transfer
0.22 μm of filter membrane, as test liquid.
3.6 take standard solution and each 10 μ L injection high performance liquid chromatograph of sample solution, peak face qualitative by retention time
Product is quantitative.
Chromatographic condition:
Chromatographic column: octadecylsilane chemically bonded silica column, 5 μm of * 4.6mm*250mm
Mobile phase: methanol: 20mmol/L ammonium acetate solution=15:85 (volume ratio)
Flow velocity: 1mL/min column temperature: 40 DEG C
Detector: diode array detector wavelength: 450nm
3.6 result judgements detect that any one of sunset yellow, lemon yellow, famille rose and Wang Jinhuang pigment can be sentenced
It is set to dried meat floss product of poor quality.
4. method validation
4.1 separating degree
Three map of spiked levels injection liquid phase high performance chromatograph is gone to be analyzed, separating degree result such as the following table 1.Standard solution
Map is shown in that Fig. 1, sample solution map are shown in Fig. 2.
Table 1
| Ingredient names | Lemon yellow | It is carmine | Sunset yellow | Wang Jinhuang |
| Separating degree | --- | 45 | 14 | 63 |
4.2 detection limits and quantitative limit
Standard solution is taken to be tested, for concentration when using signal-to-noise ratio being 3 as detection limit, concentration when signal-to-noise ratio is 10 is fixed
Amount limit, as a result such as the following table 2.
Table 2
| Ingredient names | Lemon yellow | It is carmine | Sunset yellow | Wang Jinhuang |
| Concentration (μ g/mL) | 2.311 | 2.186 | 0.981 | 1.219 |
| Signal-to-noise ratio | 68.04 | 46.27 | 40.56 | 94.18 |
| Detection limit (mg/kg) | 0.21 | 0.29 | 0.15 | 0.08 |
| Quantitative limit (mg/kg) | 0.68 | 0.95 | 0.49 | 0.26 |
3.3 ranges of linearity, are shown in Table 3.
Table 3
The range of linearity of lemon yellow: the 2.3 μ g/mL of μ g/mL~23, linearly dependent coefficient: 1.0000；
The carmine range of linearity: the 2.2 μ g/mL of μ g/mL~22, linearly dependent coefficient: 1.0000；
The range of linearity of sunset yellow: the 0.98 μ g/mL of μ g/mL~9.8, linearly dependent coefficient: 1.0000；
The range of linearity of Wang Jinhuang: the 1.2 μ g/mL of μ g/mL~12, linearly dependent coefficient: 0.9997.
4.4 precision, are shown in Table 4.
Table 4
4.5 accuracy
It respectively weighs three parts of uniformly mixed sample 10g (being accurate to 0.001g) to be placed in small beaker, is added and marks according to following table
Quasi- solution prepares test liquid according to 2.2.3, is tested, and calculates the rate of recovery, the results are shown in Table 5.
Table 5
The rate of recovery of lemon yellow is between 91.315~98.40%, and the carmine rate of recovery is 90.48%~97.37%
Between, the rate of recovery of sunset yellow between 90.29%~99.00%, the rate of recovery of Wang Jinhuang between 92.50~99.31%,
Illustration method is accurate and reliable.
4.6 sample applicabilities
In market, stochastic buying two batches dried meat floss cake and a collection of dried meat floss cake, carefully remove dried meat floss, carry out inspection in the method
Work is surveyed, wherein a batch detects to be added to sunset yellow, as a result such as the following table 6.
Table 6
Illustration method is suitable for the detection of dried meat floss sample.
Conclusion: method separation is good, and specificity is strong, and detection limit and quantitative limit are sufficiently low, and the range of linearity is good, repeatability
It is good, accurately and reliably, it can be used for day-to-day supervision detection.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of identification method of dried meat floss product of poor quality, which comprises the steps of:
Step 1: being added organic solvent into the sample of dried meat floss product and extract fat constituent therein, volatilize the organic solvent,
Collect solid phase；
Step 2: being added acetonitrile solution into the solid phase that step 1 obtains, and extracts pigment composition therein, centrifugation, collection liquid
Phase solution, the volumetric concentration of the acetonitrile solution are 70%, and the extraction pigment composition therein is will to be added to have the second
The solution of nitrile aqueous solution is ultrasonically treated, so as to be dissolved in the acetonitrile solution containing pigment composition, then is centrifuged, and described in use
Acetonitrile solution repeats to extract repeatedly the extracting liquid colourless after centrifugation, combined extract and obtains liquid solution；
Step 3: ammonium sulfate will be added after the liquid solution concentration of step 2 collection, egg therein is removed with precipitating
Liquid solution is collected in white matter ingredient, centrifugation；
Step 4: after the liquid solution that step 3 is collected is blown to net do, being transferred to polyamide solid phase extraction cartridge, therein to remove
Natural pigment ingredient collects liquid solution；
Step 5: the liquid solution collected in step 4 is blown to it is net dry, with water transfer it is fixed it is molten after cross high performance liquid chromatograph, make
Synthetic dyestuff content therein is detected with diode array detector, quantified by external standard method qualitative with retention time obtains identification knot
Fruit；
In the step 5, the condition of chromatography is:
Chromatographic column: the octadecylsilane chemically bonded silica column having a size of 5 μm of * 4.6mm*250mm；
Mobile phase: the mixed liquor for the ammonium acetate solution that the methanol and concentration that volume ratio is 15:85 are 20mmol/L；
Flow velocity: 1mL/min；
Column temperature: 40 DEG C；
Diode array detector wavelength used when detecting is 450nm.
2. the identification method of dried meat floss product of poor quality as described in claim 1, which is characterized in that in said step 1, used
Organic solvent be initial boiling point not less than 30 DEG C and the end point of distillation is not higher than 60 DEG C of petroleum ether.
3. the identification method of dried meat floss product of poor quality as described in claim 1, which is characterized in that in the step 2, described
The ultrasonic time of ultrasonic treatment is 10min.
4. the identification method of dried meat floss product of poor quality as described in claim 1, which is characterized in that in the step 2, described
The condition of centrifugation is that 10000r/min is centrifuged 5min.
5. the identification method of dried meat floss product of poor quality as described in claim 1, which is characterized in that described in the step 3
It includes: by liquid solution heating rotary evaporation concentration that ammonium sulfate will be added after the liquid solution concentration of step 2 collection
Afterwards, the ammonium sulfate that mass concentration is 10% is added while hot.
6. the identification method of dried meat floss product of poor quality as claimed in claim 5, which is characterized in that in the step 3, also wrap
It includes: the precipitating being centrifuged using water washing, then liquid solution is collected by centrifugation, and merge each centrifugate and obtain liquid solution.
7. the identification method of dried meat floss product of poor quality as described in claim 1, which is characterized in that described in the step 4
It is that the liquid solution is blown to net do using nitrogen that the liquid solution that step 3 is collected, which is blown to only dry,；
Described to be transferred to polyamide solid phase extraction cartridge, to remove natural pigment ingredient therein, collecting liquid solution includes: that will be blown to
Only after dry solution is transferred to polyamide solid phase extraction cartridge, the polyamide solid phase first is washed using the aqueous solution of 60 DEG C of pH4.0
Extraction column is multiple, then uses dehydrated alcohol-ammonium hydroxide-aqueous solution to wash colourless to stripping liquid, merges each stripping liquid and obtain liquid phase
Solution.
8. the identification method of dried meat floss product of poor quality as claimed in claim 7, which is characterized in that the aqueous solution of the pH4.0 is
The aqueous solution of ultrapure water to pH4.0 is adjusted with citric acid；
The volume ratio of dehydrated alcohol, ammonium hydroxide and water is 7:2:1 in the dehydrated alcohol-ammonium hydroxide-aqueous solution.
9. the identification method of dried meat floss product of poor quality as described in claim 1, which is characterized in that described in the step 5
The liquid solution collected in step 4 is blown to it is net dry, with water transfer it is fixed it is molten after to cross high performance liquid chromatograph include: by step 4
The liquid solution of middle collection second acid for adjusting pH to 7.0 blows steaming to net dry using nitrogen, with water transfer it is fixed it is molten after cross high-efficient liquid phase color
Spectrometer.
10. the identification method of dried meat floss product of poor quality as claimed in claim 9, which is characterized in that in the step 5, also wrap
Include by water transfer it is fixed it is molten after obtained solution cross 0.22 μm of membrane filtration the step of, the solution conduct obtained after filtering is excessively described
The test liquid of high performance liquid chromatograph.
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