CN105891350A - Method for rapidly detecting content of basic group in food - Google Patents
Method for rapidly detecting content of basic group in food Download PDFInfo
- Publication number
- CN105891350A CN105891350A CN201610190868.1A CN201610190868A CN105891350A CN 105891350 A CN105891350 A CN 105891350A CN 201610190868 A CN201610190868 A CN 201610190868A CN 105891350 A CN105891350 A CN 105891350A
- Authority
- CN
- China
- Prior art keywords
- food
- extraction element
- detection
- liquid
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid 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)
- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a method for rapidly detecting the content of a basic group in food. An integrated device is adopted, and all processes such as digestion and degradation, interfering substance precipitation, target constituent isolation and detection and analysis can be completed. Compared with the existing multi-device and multi-link treatment technologies, the method for rapidly detecting the content of the basic group in the food is obviously improved with respect to detection precision, operational convenience, detection efficiency and the like and has the advantages that work intensity is alleviated, and the space occupied by devices is saved; when the method is used for detecting a great number of detection articles, higher rapidness and convenience are achieved. By means of the rapid and accurate detection method, on one hand, enterprises and consumers can know about information of the purine content in the food, the situation that diseases such as gout and hyperuricemia are induced due to excessive intake of the human body is avoided, and the national health level is raised; on the other hand, nucleotide and basic group type products serve as important raw materials of food and pharmaceutical industries, as a result of improvement of the detection technology, the food manufacturing level and food safety guarantee level can be pushed to be raised, and it is helpful to promote economic development and social harmony at the same time.
Description
Technical field
The present invention relates to chemical analysis technology field, be specifically related to base in a kind of quickly detection food (various purine with
Pyrimidine) method of content, it is adaptable to base contents analyzes the operations such as the Specimen eliminating of process, extracting and developing, detection.
Background technology
The purine rich content of nucleic acid, nucleotides and analyte base, mankind's Excess free enthalpy will induce gout, high lithemia
The generation of the diseases such as mass formed by blood stasis, has a strong impact on the health of human kidney, extremities joint.But at present, along with the development increasing fresh technology
With universal, Partial Food enterprise, for improving mouthfeel and delicate flavour, arbitrarily adds guanylic acid and inosinicacid (I+G), yeast in food
Extract, seafood extract contour purine thing, and in food labelling, do not make mark in detail.Therefore it provides it is a kind of quick
With the technology of purine content in accurately detection food, allow business and consumer grasp food purine content information, the mankind are improved
The disease-resistant level that keeps healthy has important Practical significance.Nucleotides, base series products be also food and medicinal industry important source material it
One, improving promoting food manufacturing level, the raising of food security safeguard level of detection technique, may advantageously facilitate economic development
With social harmony.
Owing to the nucleic acid of most products, nucleotides, base (purine and pyrimidine) are often combined with other compositions or coexist,
Detection sample needs first to carry out strong acid decomposition, acid-base neutralization, sex change precipitation etc. and processes, and is extracted by target component and detects, therefore
Multiple preprocessing means need to be used to reduce nucleic acid, remove albumen, the interference component such as polysaccharide, product auxiliary material, byproduct of reaction.But
In existing conventional isolation techniques, every kind of preprocessing means can only use the utensil of correspondence, such as digestion degraded, chemically derived operation one
As with digestion tube, derivative pipe, impurity (active ingredient) adsorbs or precipitate and uses beaker, flask or reactor;Lock out operation uses
Funnel, filter etc.., when processing a large amount of inspection product or step complexity, often there is substantial amounts of device in these customary furnishings function singlenesses
Tool needs use and with after need cleaning, utensil takies in working space, complex operation, link switching process occurs that Liquid Residue damages
Lose or the problems such as the improper dilution of sample, resulted in the defects such as detection working strength is big, efficiency is low, detection error is big or
Not enough.
Therefore, for the problems referred to above, the invention provides one and utilize this integrated apparatus to realize in quick detection food
The method of base contents, by utilizing Multifunctional inspection sample extraction separator, can significantly improve in complex biochemical product
Base contents detection efficiency, reduce processing links and required multiple utensil, reduce conventional method need to process through many appliances,
Shift and cause sample loss or make the detection error being diluted to;Further, the present invention also has reduction labour intensity, improves detection
The degree of accuracy, when a large amount of sample detection, more has and processes the advantage quick, efficiency is high.
Summary of the invention
The invention provides and quickly detect the method for base contents in food, it is adaptable to detection food nucleotide, base
Pretreatment such as the clearing up of sample, extracting and developing and analyze operation.
In order to realize the technical purpose of the present invention, the present invention adopts the following technical scheme that.
A kind of method of base contents in quick detection food, uses Multifunctional inspection sample extraction separator, specifically
Comprise the steps:
A () clears up reaction: be sequentially added into the thing to be detected after dilution, perchloric acid in reaction unit, mix, be filled with inertia
Gas, after sealing with sealed bolster plate, fasten the first quick clip, adds thermal response 20 ~ 60 minutes;
B () extracts: open the first quick clip and sealed bolster plate, pour in extraction element by the reactant liquor in reaction unit, this
Time, the bottom of extraction element is for sealing structure;With a small amount of pure water reaction unit two times, and proceed to cleaning solution extract dress
Put, under stirring, with strong base solution regulation reacting liquid pH value to 7.0, stand 10 minutes;
C () filters: open the second quick clip, along spacing rubber gasket, the bottom direction axial tension sump assemblies of hex bolts,
Utilize negative pressure by the filter media in telescopic chute of the extract after alkaline solution treatment to device for storing liquid, and another container is received
Collection extracts filtrate;
D () washing is collected: device for storing liquid top of pulling back is to closing filter bores in the middle part of telescopic chute, after fastening the second quick clip,
Add a small amount of pure water extraction element and sediment in extraction element, repeat step (c) and cleaning solution is proceeded in the lump step
In the container of (c), obtain mixed liquor after mixing, and be settled to certain volume (adjusting with pure water) with volumetric flask, make sample
Product test liquid;
E () is analyzed: by molten for sample test liquid filtering with microporous membrane, contained fast in analytical solution in injection high performance liquid chromatograph
The base contents such as purine, pyrimidine, analysis condition: use octadecylsilane chemically bonded silica, UV-detector, UV-detector, etc.
Degree or gradient elution;
Wherein, described Multifunctional inspection sample extraction separator is integrated, including reaction unit, extraction element, storage
Liquid device, is positioned at the valve bottom device for storing liquid, and valve is circumscribed with valve adapter, is arranged on described reaction unit and extracts dress
Sealed bolster plate between putting, is also associated with H shape shape telescopic chute, the middle part of telescopic chute between described extraction element and device for storing liquid
Being provided with multiple perforate and projection, the lower end of described telescopic chute is provided with spacing rubber gasket, axially may be used along spacing rubber gasket direction
Telescopic filter unit, be disposed with between described extraction element and device for storing liquid fluid sealant packing ring, filter medium, telescopic chute and
U-shaped rubber gasket, described U-shaped rubber gasket is provided with multiple conduction hole.
Preferably, in described step (a), the mass concentration of thing to be detected is 1% ~ 5%, and dilution is pure water.
Preferably, in described step (a), the volume ratio of thing solution to be detected and perchloric acid solution is 1:1 ~ 2.
Preferably, being filled with inert gas in described step (a) is in nitrogen, helium, neon, argon gas, Krypton, xenon
Kind.
Preferably, in described step (a), heating-up temperature is 90 DEG C ~ 120 DEG C, and pressure is 0 ~ 103.4kPa, (1.05kg/
cm2).
Preferably, in described step (b), strong base solution is in NaOH, potassium hydroxide or lithium hydroxide solution
Kind.
Preferably, in described step (b), strong base solution concentration is 1mol/L ~ 20 mol/L.
It is furthermore preferred that strong base solution concentration is 1mol/L ~ 10 mol/L in described step (b).
Preferably, the filter medium in described step (c) is the one in screen cloth, filter paper or filter membrane.
The invention have the advantages that: the invention provides and quickly detect the method for base contents in food, pass through
Use integrated apparatus, whole mistakes such as digestion degraded, interfering material precipitation, target component separation, detection analysis can be completed in the lump
Journey.
Compared with prior art, the method for base contents in the quickly detection food that the present invention provides, either
In accuracy of detection, in terms of simple operation, or reducing analytical error, saving the utensil aspect that takes up room and all have significantly
Progress, overcome the deficiency of conventional method.
Accompanying drawing explanation
For the technical scheme being illustrated more clearly that in the embodiment of the present invention, in embodiment being described below required for make
Accompanying drawing be briefly described:
Fig. 1 is that the present invention reacts or extracts status architecture schematic diagram;
Fig. 2 is filtration condition structural representation of the present invention;
Fig. 3 is perforate schematic diagram on telescopic chute flat board of the present invention;
Fig. 4 is conduction hole schematic diagram on U-shaped rubber gasket of the present invention.
Fig. 5 is the present invention spacing rubber gasket schematic diagram.
In figure: 1-reaction unit;11-sealed bolster plate;2-extraction element;21-filter medium;3-device for storing liquid;31-valve
Door;32-valve is taken over;4-telescopic chute;41-perforate;42-is protruding;51-the first Quick hoop;52-the second Quick hoop;61-is close
Sealing packing ring;The spacing rubber gasket of 62-;63-U shape rubber gasket;64-conduction hole;71-hex bolts one;72-hex bolts two.
Detailed description of the invention
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearer, below in conjunction with
Drawings and Examples, are further elaborated to the present invention.Should be appreciated that specific embodiment described herein is only used
To explain the present invention, do not limit the present invention.
With reference to shown in Fig. 1, Fig. 2, Fig. 3, Fig. 4 and Fig. 5, a kind of Multifunctional inspection sample extraction separator, including device
Main body, described apparatus main body includes superposed reaction unit 1, the extraction element 2 at middle part and the device for storing liquid 3 of bottom, position
Valve 31 bottom device for storing liquid 3, connects fixing reaction unit 1 and the first Quick hoop 51 of extraction element 2, connects fixing
Extraction element 2 and the second Quick hoop 52 of device for storing liquid 3, be provided with sealing gasket between described reaction unit 1 and extraction element 2
Plate 11, connects between described extraction element 2 and device for storing liquid 3 and has telescopic chute 4, the lower end of described telescopic chute 4 to be provided with spacing glue
Packing ring 62, is disposed with fluid sealant packing ring 61, filter medium 21, telescopic chute 4 between described extraction element 2 and device for storing liquid 3
With U-shaped rubber gasket 63, described apparatus main body passes through the first Quick hoop 51 and the second Quick hoop 52 by reaction unit 1, extraction
Device 2 and device for storing liquid 3 connect as one structure.
Described telescopic chute 4 is H shape shape, and the middle part of telescopic chute 4 is the slab construction being provided with multiple perforate 41.Described storage
Being provided with 8-16 conduction hole 64 on U-shaped rubber gasket 63 within liquid device 3, described conduction hole 64 is positioned at the periphery of perforate 41,
The middle part of described telescopic chute 4 is provided with the projection 42 of the sealing corresponding with conduction hole 64 of equal number.Described filter medium 21 is
One in screen cloth, filter paper or filter membrane.The top of described telescopic chute 4 is additionally provided with the hex bolts one that 4-10 each and every one strengthens fixing
71, the bottom of described telescopic chute 4 is provided with 4-10 and strengthens fixing hex bolts 2 72, and described hex bolts 2 72 is through limit
Position rubber gasket 62 also screws in telescopic chute formation connection with threaded engagement.Described device for storing liquid 3 is along spacing rubber gasket 62, hexagonal
Bolt 2 72 direction axial stretching, is further connected with valve adapter 32 on described valve 31.
Further below the Multifunctional inspection sample extraction separator in the present invention is described in detail.
Reaction unit 1 is responsible for Specimen eliminating function, by being arranged on the sealing gasket between reaction unit 1 and extraction element 2
Plate 11 seals, and after loading onto the first Quick hoop 51, stands upside down and place, as Specimen eliminating device, can be used for various strong acid, highly basic and
Chemical breakdown (deriving) under the conditions of neutrality gentleness etc. or biological enzymatic decomposition (deriving), decompose Applicable temperature and be 0-125 DEG C, fit
With pressure less than 103.4kPa(1.05kg/cm2).After having reacted, open the first Quick hoop 51, sealed bolster plate 11, can
Carry out the operations such as the stopping of reaction of next step flow process, soda acid adjustment, organic solvent deposit, sex change, extraction or adsorption treatment.
Extraction element 2 and device for storing liquid 3 are responsible for extraction and the filtering function of device.Extraction element 2 and sump assemblies 3 are
Cylindrical shape, by with telescopic chute on 4 hex bolts 1, hex bolts 2 72 be fastenedly connected integral.The middle part of telescopic chute 4
Being provided with the projection 42 of sealing corresponding with conduction hole 64, protruding 42 just seal up the conduction hole 64 on U-shaped rubber gasket 63, will carry
Fetching puts the sealed bottom of 2.Now, between extraction element 2 and device for storing liquid 3, it is in state of isolation, can enter in extraction element 2
The subsequent extracted of row sample or solid cleaning, release protruding 42 and be engaged with the sealing of U-shaped rubber gasket 63, realize the most further
Liquid filtering function.
After pulling down the second Quick hoop 52 of connection extraction element 2 and sump assemblies 3, can be by sump assemblies 3 along spacing glue
Packing ring 62, the bottom direction axial tension of hex bolts 2 72, maximum tension distance is to support to six to 62 times edges of spacing rubber gasket
The upper edge of corner bolt 2 72.By sump assemblies 3 is stretched, make the inner space of device for storing liquid 3 become big, produce local decompression,
And then make the liquid in extraction element 2 filter to bottom sump assemblies 3, it is achieved filtering function.Further, device for storing liquid 3 is closed
Bottom valve 31, and by device for storing liquid 3 along maximum tension distance pull back to extraction element 2 time, now, by device for storing liquid 3
The local malleation that process of pulling back produces, makes gas escape from the side of device for storing liquid 3 to the side of extraction element 2, and then impact
Deposit on filter medium 21, reversely dredges filter medium 21, it is achieved strainability improves or realizes at the beginning of filter medium
Step cleaning.
In the Multifunctional inspection sample extraction separator that the present invention provides, digestion degraded, impurity (active ingredient) are inhaled
Attached or the processing links such as precipitation, liquid or solid separation completes in same set of device.This integrated design device has structure
The compactest, good airproof performance, mobile smooth and easy, stable and reliable for performance, multiple functional, installing/dismounting is quick, easy to clean etc. multiple
Advantage, can be according to processing intent flexible combination device, due to the reaction unit 1 of different capabilities, extraction element 2, telescopic chute 4, storage
It is consistent that liquid device 3 engages bore specification, and docking is identical.Significantly reduce and artificially detect error, improve detection efficiency, change
Operating environment and working condition are apt to it.Apparatus of the present invention main body is made up of stainless steel, glass or similar material, metal material anti-
The lining material answering device 1 inner surface is PTFE-polytetrafluoroethylene (PTFE), strengthens this device acid and alkali-resistance, oxidant, organic solvent corrosion
With high temperature resistant, high-voltage performance.
The purine in food, pyrimidine etc. are carried out below as a example by food yeast powder, yeast extract, broken wall type food yeast
The rapid and accurate determination of base, but be not regarded as limiting of the invention, present disclosure additionally applies for such as seafood food, beans system
The base contents detection of the food such as product, pickles.
Embodiment 1
A kind of method of base contents in quick detection food yeast powder, uses the Multifunctional inspection sample extraction that the present invention provides
Separator, specifically includes following steps:
A () clears up reaction: being sequentially added into 5ml mass fraction in reaction unit is 1% food yeast amidin and 5ml height chlorine
Acid, mixes, and is filled with nitrogen, after sealing with sealed bolster plate, fasten the first quick clip, and heating in water bath for reaction 60 at 100 DEG C
Minute;
B () extracts: open the first quick clip and sealed bolster plate, pour in extraction element by the reactant liquor in reaction unit, this
Time, the bottom of extraction element is for sealing structure;With a small amount of pure water reaction unit two times, and proceed to cleaning solution extract dress
Put, under stirring, with the potassium hydroxide solution regulation reacting liquid pH value of 10mol/L to 7.0, stand 10 minutes;
C () filters: open the second quick clip, along spacing rubber gasket, the bottom direction axial tension sump assemblies of hex bolts,
Extract after utilizing negative pressure to stand filters to device for storing liquid, and another container collection extracts filtrate;
D () washs: device for storing liquid top of pulling back, to closing filter bores in the middle part of telescopic chute, is loaded onto the second quick clip and fastens.?
Add a small amount of pure water extraction element and sediment in extraction element, repeat step (c) and cleaning solution is proceeded in the lump step
In the container of (c), after mixing, obtain mixed liquor, with volumetric flask, mixed liquor be settled to certain volume (adjusting with pure water),
Make sample test liquid;
E () is analyzed: by sample test liquid with 0.45 micrometer Millipore membrane filtration, inject high performance liquid chromatograph analysis sample molten
Institute's base contents such as purine-containing, pyrimidine in liquid.Analysis condition: Agilent 1100 high performance liquid chromatograph;Chromatographic column:
HypersilBDS-C18,5 μ, 4.6mmx250mm;Flowing phase: 0.2mol/L phosphate buffer;Column temperature: 30 DEG C;Detection ripple
Long: 254nm, flow velocity: 1.0ml/ minute.
F () inventive method compares with the measurement result of conventional method
With reference to embodiment 1, use conventional independent utensil to process detection sample, obtain the sample test liquid arrived, inject efficiently
Base contents analyzed by liquid chromatograph, is designated as comparative example 1.Two kinds of method test comparison results are as shown in table 1.
The table 1 food yeast powder measurement result table of comparisons (mean value ± SD% measures 3 times, content unit mg/g)
Project | Cytimidine | Uracil | Guanine | Adenine | Inspection product pretreatment time (average/time) |
Embodiment 1 | 2.94±2.38% | 5.22±3.26% | 6.30±2.94% | 7.70±3.01% | 82.6 minutes |
Comparative example 1 | 3.05±4.84% | 4.63±4.37% | 6.52±4.87% | 6.44±5.03% | 107.8 minute |
Embodiment 2
A kind of method of base contents in quick detection yeast extract, uses the Multifunctional inspection sample extraction that the present invention provides
Separator, specifically includes following steps:
A () clears up reaction: being sequentially added into 5ml mass fraction in reaction unit is the 5% yeast extract aqueous solution and 10ml height chlorine
Acid, mixes, and is filled with nitrogen, after sealing with sealed bolster plate, fasten the first quick clip, adds thermal response 20 minutes at 120 DEG C;
B () extracts: open the first quick clip and sealed bolster plate, pour in extraction element by the reactant liquor in reaction unit, this
Time, the bottom of extraction element is for sealing structure;With a small amount of pure water reaction unit two times, and proceed to cleaning solution extract dress
Put, under stirring, with the sodium hydroxide solution regulation reacting liquid pH value of 1mol/L to 7.0, stand 10 minutes;
C () filters: open the second quick clip, along spacing rubber gasket, the bottom direction axial tension sump assemblies of hex bolts,
Extract after utilizing negative pressure to stand filters to device for storing liquid, and another container collection extracts filtrate;
D () washs: device for storing liquid top of pulling back, to closing filter bores in the middle part of telescopic chute, is loaded onto the second quick clip and fastens.?
Add a small amount of pure water extraction element and sediment in extraction element, repeat step (c) and cleaning solution is proceeded in the lump step
In the container of (c), after mixing, obtain mixed liquor, with volumetric flask, mixed liquor be settled to certain volume (adjusting with pure water),
Make sample test liquid;
E () is analyzed: by molten for sample test liquid with 0.45 micrometer Millipore membrane filtration, inject high performance liquid chromatograph and analyze sample
Institute's base contents such as purine-containing, pyrimidine in solution.Analysis condition: Agilent 1100 high performance liquid chromatograph;Chromatographic column:
HypersilBDS-C18,5 μ, 4.6mmx250mm;Flowing phase: 0.2mol/L phosphate buffer;Column temperature: 30 DEG C;Detection ripple
Long: 254nm, flow velocity: 1.0ml/ minute.
F () inventive method compares with the measurement result of conventional method
With reference to embodiment 2, use conventional independent utensil to process detection sample, obtain the sample test liquid arrived, inject efficiently
Base contents analyzed by liquid chromatograph, is designated as comparative example 2.Two kinds of method test result comparisons are as shown in table 2.
The table 2 yeast extract measurement result table of comparisons (mean value ± SD% measures 3 times, content unit mg/g)
Project | Cytimidine | Uracil | Guanine | Adenine | Inspection product pretreatment time (average/time) |
Embodiment 2 | 3.58±3.54% | 6.08±2.11% | 7.93±1.42% | 8.84±2.75% | 40.8 minutes |
Comparative example 2 | 3.43±4.09% | 5.58±4.34% | 7.72±3.74% | 7.46±4.81% | 65.1 minutes |
Embodiment 3
A kind of method of base contents in quick detection broken wall type food yeast, uses the Multifunctional inspection sample that the present invention provides
Extract separator, specifically include following steps:
A () clears up reaction: being sequentially added into 5ml mass fraction in reaction unit is 5% broken wall type food yeast and 10ml height chlorine
Acid, mixes, and is filled with nitrogen, with sealed bolster plate seal, after fastening the first quick clip, 100 DEG C of heating in water bath for reaction 30 points
Clock;
B () extracts: open the first quick clip and sealed bolster plate, pour in extraction element by the reactant liquor in reaction unit, this
Time, the bottom of extraction element is for sealing structure;With a small amount of pure water reaction unit two times, and proceed to cleaning solution extract dress
Put, under stirring, with the lithium hydroxide solution regulation reacting liquid pH value of 20mol/L to 7.0, stand 10 minutes;
C () filters: open the second quick clip, along spacing rubber gasket, the bottom direction axial tension sump assemblies of hex bolts,
Extract after utilizing negative pressure to stand filters to device for storing liquid, and another container collection extracts filtrate;
D () washing is collected: the second quick clip, to closing filter bores in the middle part of telescopic chute, is loaded onto the tightest in device for storing liquid top of pulling back
Gu.In extraction element, add a small amount of pure water extraction element and sediment, repeat step (c) and cleaning solution is proceeded in the lump
In the container of step (c), obtain mixed liquor after mixing, and be settled to certain volume with volumetric flask, make sample test liquid;
E () is analyzed: by molten for sample test liquid with 0.45 micrometer Millipore membrane filtration, inject high performance liquid chromatograph and analyze sample
Institute's base contents such as purine-containing, pyrimidine in solution.Analysis condition: Agilent 1100 high performance liquid chromatograph;Chromatographic column:
HypersilBDS-C18,5 μ, 4.6mmx250mm;Flowing phase: 0.2mol/L phosphate buffer;Column temperature: 30 DEG C;Detection ripple
Long: 254nm, flow velocity: 1.0ml/ minute.
F () inventive method compares with the measurement result of conventional method
With reference to embodiment 3, use conventional independent utensil to process detection sample, obtain the sample test liquid arrived, inject with method
Base contents analyzed by high performance liquid chromatograph, is designated as comparative example 3.Two kinds of method test result comparisons are as shown in table 3.
The table 3 base contents measurement result table of comparisons (mean value ± SD% measures 3 times, content unit mg/g)
Project | Cytimidine | Uracil | Guanine | Adenine | Inspection product pretreatment time (average/time) |
Embodiment 1 | 2.97±3.12% | 5.41±4.44% | 5.87±3.78% | 7.81±4.08% | 52.1 minutes |
Comparative example 1 | 2.74±7.48% | 5.09±6.00% | 6.22±7.32% | 7.42±8.03% | 80.3 minutes |
According to upper table data it can be seen that compare with existing Technology development, in the quickly detection food that the present invention provides
The method of base contents, in accuracy of detection, error degree reduces about 50%, shortens to original 65%, precision on the detection time
Substantially improve with the sample pretreatment time, the most more save the feature of utensil, more convenient and quicker simultaneously.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment done within god and principle, equivalent etc., should be included within the scope of the present invention.
Claims (8)
1. the method for base contents in a quick detection food, it is characterised in that use Multifunctional inspection sample extraction to separate
Device, specifically includes following steps:
A () clears up reaction: be sequentially added into the thing to be detected after dilution, perchloric acid in reaction unit, mix, be filled with inertia
Gas, after sealing with sealed bolster plate, fasten the first quick clip, adds thermal response 20 ~ 60 minutes;
B () extracts: open the first quick clip and sealed bolster plate, pour in extraction element by the reactant liquor in reaction unit, this
Time, the bottom of extraction element is for sealing structure;With a small amount of pure water reaction unit two times, and proceed to cleaning solution extract dress
Put, under stirring, with strong base solution regulation reacting liquid pH value to 7.0, stand 10 minutes;
C () filters: open the second quick clip, and the bottom direction axial tension reservoir along spacing rubber gasket, hex bolts two fills
Put, the extract after utilizing negative pressure reaction to be stood, through filter media to device for storing liquid, and separately extract filter with container collection
Liquid;
D () washing is collected: device for storing liquid top of pulling back is to closing filter bores in the middle part of telescopic chute, after fastening the second quick clip.
2. in extraction element, add a small amount of pure water extraction element and sediment, repeat step (c) by cleaning solution in the lump
Proceed to, in the container of step (c), obtain mixed liquor after mixing, and be settled to certain volume with volumetric flask, make sample and supply
Test solution;
E () is analyzed: by molten for sample test liquid filtering with microporous membrane, contained fast in analytical solution in injection high performance liquid chromatograph
The base contents such as purine, pyrimidine;
Wherein, described Multifunctional inspection sample extraction separator is integrated, including reaction unit, extraction element, storage
Liquid device, is positioned at the valve bottom device for storing liquid, and valve is circumscribed with valve adapter, is arranged on described reaction unit and extracts dress
Sealed bolster plate between putting, is also associated with H shape shape telescopic chute, the middle part of telescopic chute between described extraction element and device for storing liquid
Being provided with multiple perforate and projection, the lower end of described telescopic chute is provided with spacing rubber gasket, axially may be used along spacing rubber gasket direction
Telescopic filter unit, be disposed with between described extraction element and device for storing liquid fluid sealant packing ring, filter medium, telescopic chute and
U-shaped rubber gasket, described U-shaped rubber gasket is provided with multiple conduction hole.
The method of base contents in a kind of quick detection food the most according to claim 1, it is characterised in that: described step
A in (), the mass fraction of thing to be detected is 1% ~ 5%, dilution is pure water.
The method of base contents in a kind of quick detection food the most according to claim 1, it is characterised in that: described step
A in (), thing solution to be detected is 1:1 ~ 2 with the volume ratio of perchloric acid solution.
The method of base contents in a kind of quick detection food the most according to claim 1, it is characterised in that: described step
A being filled with inert gas in () is the one in nitrogen, helium, neon, argon gas, Krypton, xenon.
The method of base contents in a kind of quick detection food the most according to claim 1, it is characterised in that: described step
A in (), heating-up temperature is 90 DEG C ~ 120 DEG C, pressure is 0 ~ 103.4kPa.
The method of base contents in a kind of quick detection food the most according to claim 1, it is characterised in that: described step
One b strong base solution is NaOH, potassium hydroxide or lithium hydroxide solution in () in
The method of base contents in a kind of quick detection food according to claim 1, it is characterised in that: described step
B in (), strong base solution concentration is 1mol/L ~ 20 mol/L.
The method of base contents in a kind of quick detection food the most according to claim 1, it is characterised in that: described step
The one c filter medium in telescopic chute is screen cloth, filter paper or filter membrane in () in.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610190868.1A CN105891350B (en) | 2016-03-29 | 2016-03-29 | A kind of method of base contents in quick detection food |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610190868.1A CN105891350B (en) | 2016-03-29 | 2016-03-29 | A kind of method of base contents in quick detection food |
Publications (2)
Publication Number | Publication Date |
---|---|
CN105891350A true CN105891350A (en) | 2016-08-24 |
CN105891350B CN105891350B (en) | 2018-06-05 |
Family
ID=57014708
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610190868.1A Expired - Fee Related CN105891350B (en) | 2016-03-29 | 2016-03-29 | A kind of method of base contents in quick detection food |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN105891350B (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110208076A (en) * | 2019-06-14 | 2019-09-06 | 浙江省食品药品检验研究院 | A kind of digestion instrument for amino acid resolution experiment |
CN114994265A (en) * | 2022-07-15 | 2022-09-02 | 徐州锡沂康成食品检验检测研究院有限公司 | Detection and analysis equipment for fluid food |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103235056A (en) * | 2013-04-12 | 2013-08-07 | 润德(山东)检测技术有限公司 | Method for detecting guanine and adenine in food |
-
2016
- 2016-03-29 CN CN201610190868.1A patent/CN105891350B/en not_active Expired - Fee Related
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103235056A (en) * | 2013-04-12 | 2013-08-07 | 润德(山东)检测技术有限公司 | Method for detecting guanine and adenine in food |
Non-Patent Citations (3)
Title |
---|
H. FAN ET AL.: "Determination of purine and pyrimidine bases in natural and cultured Cordyceps using optimum acid hydrolysis followed by high performance liquid chromatography", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
刘桂英 等: "豆类中4种嘌呤的高效液相色谱测定法", 《中国卫生检验杂志》 * |
杨海斌 等: "高效液相色谱法同时测定肉类食品中的嘌呤和尿酸", 《卫生研究》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110208076A (en) * | 2019-06-14 | 2019-09-06 | 浙江省食品药品检验研究院 | A kind of digestion instrument for amino acid resolution experiment |
CN110208076B (en) * | 2019-06-14 | 2021-10-12 | 浙江省食品药品检验研究院 | Digestion device for amino acid digestion experiment |
CN114994265A (en) * | 2022-07-15 | 2022-09-02 | 徐州锡沂康成食品检验检测研究院有限公司 | Detection and analysis equipment for fluid food |
Also Published As
Publication number | Publication date |
---|---|
CN105891350B (en) | 2018-06-05 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
WO2007002580A3 (en) | Diagnostic as say system with multi -well reagent container | |
CN101334365B (en) | Determination method for chloride ion content of temper rolling liquor for steel plate rolling | |
CN105891350A (en) | Method for rapidly detecting content of basic group in food | |
CN105044262A (en) | Water polychlorinated biphenyl dispersive solid-phase extraction gas chromatography detection method | |
CN106841447A (en) | A kind of VPCE static properties method of testing | |
CN205719681U (en) | A kind of Multifunctional inspection sample extraction segregation apparatus | |
CN103983636B (en) | A kind of sulfate reducting bacteria method for quick and test kit thereof | |
CN105675371B (en) | A kind of Multifunctional inspection sample extraction separator | |
Frenzel | Microanalytical concept for multicomponent analysis of airborne particulate matter | |
CN101122608A (en) | Chemical treatment cartridge and method of using same | |
CN106596765A (en) | Method for detecting addition amount of maltodextrin in food materials | |
CN205981835U (en) | Processor before chemical analysis sample is synthesized | |
CN210078908U (en) | Integrated solid phase extraction column | |
CN105334072B (en) | A kind of sealed fecal sample sampling container and sampling method | |
CN207980505U (en) | A kind of solid-phase extraction device | |
CN206431144U (en) | A kind of portable clenbuterol hydrochloride assay kit | |
CN103100363B (en) | Automatic derivatization reaction processing equipment and method | |
CN109796702B (en) | Preparation method of PVC fluorescent film | |
CN206459882U (en) | A kind of Sample Purification on Single reaction tube | |
CN103454135A (en) | Device for combining sample enrichment with analytical instrument | |
CN206270130U (en) | The sample pretreatment device of organic carbon content test experiments | |
CN205786536U (en) | Portable test kit | |
CN205216257U (en) | High pressure solvent extraction pond | |
TW200736610A (en) | Biochemical reaction cassette and analytical method using the same | |
CN218046592U (en) | Accurate control solid phase extraction device |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180605 Termination date: 20190329 |