CN114636766B - Application of reagent taking mechanism in detecting food pantothenic acid - Google Patents
Application of reagent taking mechanism in detecting food pantothenic acid Download PDFInfo
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- CN114636766B CN114636766B CN202210225695.8A CN202210225695A CN114636766B CN 114636766 B CN114636766 B CN 114636766B CN 202210225695 A CN202210225695 A CN 202210225695A CN 114636766 B CN114636766 B CN 114636766B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
Abstract
The invention discloses a rapid detection reagent for pantothenic acid in food, which comprises 0.05-0.25 mol/L hydrochloric acid, 0.3-0.5 mol/L zinc sulfate solution, 0.01-0.05 mol/L potassium dihydrogen phosphate solution and 1-2 mg/L D-calcium pantothenate solution; above-mentioned solution holds in reagent takes mechanism, reagent takes mechanism includes the casing, the top cap that can open and shut is installed at the casing top, refrigeration compressor and the refrigeration coil who is connected with refrigeration compressor are installed to the casing bottom, a plurality of reagent transparent storage tank is installed at the casing top in the top cap, the surface of reagent transparent storage tank is provided with the scale, detachable sealing plug is installed at reagent transparent storage tank top, be fixed with flexible trachea on the sealing plug, flexible tracheal one end is located reagent transparent storage tank, flexible tracheal other end is connected with the nitrogen gas jar, titration valve is installed to reagent transparent storage tank's lateral wall bottom. The invention can improve the defects of the prior art and realize long-term safe storage and rapid proportioning use of the reagent.
Description
Technical Field
The invention relates to the technical field of food detection, in particular to application of a reagent taking mechanism in detecting food pantothenic acid.
Background
The determination of pantothenic acid in food is an important item in food testing. Because the detection process requires multiple reagents, it takes much time to configure and take each time before detection.
Disclosure of Invention
The technical problem to be solved by the invention is to provide an application of a reagent taking mechanism in detecting food pantothenic acid, so that long-term safe storage and rapid proportioning use of the reagent are realized.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows.
A rapid detection reagent for pantothenic acid in food:
comprises 0.05 to 0.25mol/L hydrochloric acid, 0.3 to 0.5mol/L zinc sulfate solution, 0.01 to 0.05mol/L monopotassium phosphate solution and 1 to 2mg/L D-calcium pantothenate solution;
above-mentioned solution holds in reagent takes mechanism, reagent takes mechanism includes the casing, the top cap that can open and shut is installed at the casing top, refrigeration compressor and the refrigeration coil who is connected with refrigeration compressor are installed to the casing bottom, a plurality of reagent transparent storage tank is installed at the casing top in the top cap, the surface of reagent transparent storage tank is provided with the scale, detachable sealing plug is installed at reagent transparent storage tank top, be fixed with flexible trachea on the sealing plug, flexible tracheal one end is located reagent transparent storage tank, flexible tracheal other end is connected with the nitrogen gas jar, titration valve is installed to reagent transparent storage tank's lateral wall bottom.
Preferably, the aqueous solution comprises 0.1mol/L hydrochloric acid, 0.5mol/L zinc sulfate solution, 0.02mol/L potassium dihydrogen phosphate solution and 1mg/L D-calcium pantothenate solution.
Preferably, the titration valve comprises a valve body, a valve cavity is arranged in the valve body, a liquid inlet hole communicated with the reagent transparent storage tank is formed in the side wall of the valve cavity, a liquid outlet hole is formed in the side wall of the valve cavity, a dropper is connected to the outer side of the liquid outlet hole, a switch valve is respectively arranged at the liquid inlet end of the liquid inlet hole and the liquid outlet end of the liquid outlet hole, a partition plate is movably arranged in the valve cavity, a sealing ring in sealing contact with the valve cavity is arranged at the edge of the partition plate, a fine adjustment screw is arranged on the valve body, one end of the fine adjustment screw is connected with the partition plate, and the other end of the fine adjustment screw is positioned at the outer side of the valve body.
Preferably, the dropper is disposed obliquely downward.
Preferably, the side wall of the dropper is provided with a bypass pipe, and the bypass pipe is provided with a switch valve.
The preparation method of the reagent for rapidly detecting pantothenic acid in food comprises the following steps:
A. placing concentrated hydrochloric acid stock solution into a volumetric flask, and adding water to dilute the stock solution to 1000mL;
B. taking zinc sulfate heptahydrate, adding water for dissolution and fixing the volume to 100mL;
C. dissolving potassium dihydrogen phosphate in water, adjusting pH to 3.0 with phosphoric acid, diluting to 1000mL with water, and filtering with 0.45 μm filter membrane;
D. taking a D-calcium pantothenate solution, adding water to fix the volume to 1000mL;
E. and D, removing the sealing plug, placing the solution prepared in the steps A-D into a reagent transparent storage tank, and then re-covering the sealing plug for later use.
The application of the reagent for rapidly detecting pantothenic acid in food in detecting pantothenic acid in food.
Preferably, the detection method is liquid chromatography.
The beneficial effects brought by adopting the technical scheme are as follows: the invention can configure the used reagent in advance, store the reagent in the reagent taking mechanism at low temperature, take the reagent rapidly and accurately according to the requirement when detecting, and save the detection time.
Drawings
FIG. 1 is a block diagram of a reagent dispensing mechanism according to one embodiment of the present invention.
FIG. 2 is a block diagram of a titration valve in an embodiment of the invention.
In the figure: 1. a housing; 2. a top cover; 3. a refrigeration compressor; 4. a refrigeration coil; 5. a reagent transparent storage tank; 6. a sealing plug; 7. a flexible air tube; 8. a nitrogen tank; 9. a titration valve; 10. a valve body; 11. a valve cavity; 12. a liquid inlet hole; 13. a liquid outlet hole; 14. a dropper; 15. a switch valve; 16. a partition plate; 17. a seal ring; 18. fine tuning the screw; 19. and a bypass tube.
Detailed Description
Referring to FIGS. 1-2, a rapid detection reagent for pantothenic acid in a food product comprises 0.1mol/L hydrochloric acid, 0.5mol/L zinc sulfate solution, 0.02mol/L potassium dihydrogen phosphate solution, 1mg/L D-calcium pantothenate solution;
above-mentioned solution holds in reagent takes mechanism, reagent takes mechanism includes casing 1, casing 1 installs top cap 2 that can open and shut at the top, refrigeration compressor 3 and the refrigeration coil 4 of being connected with refrigeration compressor 3 are installed to casing 1 bottom, a plurality of reagent transparent storage tank 5 are installed at casing 1 top in the top cap 2, the surface of reagent transparent storage tank 5 is provided with the scale, detachable sealing plug 6 is installed at reagent transparent storage tank 5 top, be fixed with flexible trachea 7 on the sealing plug 6, one end of flexible trachea 7 is located reagent transparent storage tank 5, the other end and the nitrogen gas jar 8 of flexible trachea 7 are connected, titration valve 9 is installed to the lateral wall bottom of reagent transparent storage tank 5. The titration valve 9 comprises a valve body 10, a valve cavity 11 is arranged in the valve body 10, a liquid inlet hole 12 communicated with the reagent transparent storage tank 5 is arranged on the side wall of the valve cavity 11, a liquid outlet hole 13 is arranged on the side wall of the valve cavity 11, a dropper 14 is connected to the outer side of the liquid outlet hole 13, a switch valve 15 is respectively arranged at the liquid inlet end of the liquid inlet hole 12 and the liquid outlet end of the liquid outlet hole 13, a partition plate 16 is movably arranged in the valve cavity 11, a sealing ring 17 in sealing contact with the valve cavity 11 is arranged at the edge of the partition plate 16, a fine adjustment screw 18 is arranged on the valve body 10, one end of the fine adjustment screw 18 is connected with the partition plate 16, and the other end of the fine adjustment screw 18 is positioned at the outer side of the valve body 10. The drip tube 14 is disposed obliquely downward. The side wall of the dropper 14 is provided with a bypass pipe 19, and the bypass pipe 19 is provided with an on-off valve 15.
When the reagent is taken, the switch valve 15 on the liquid outlet hole 13 is kept closed, the switch valve 15 on the liquid inlet hole 12 is opened, then the fine adjustment screw 18 is rotated according to the taken amount, along with the movement of the partition plate 16, the reagent flows into the valve body 10 from the reagent transparent storage tank 5, then the switch valve 15 on the liquid outlet hole 13 is opened, the switch valve 15 on the liquid inlet hole 12 is closed, the fine adjustment screw 18 is rotated in the opposite direction, the partition plate 16 pushes the reagent, and the reagent flows out from the dropper 14.
The valve chamber 11 can be conveniently flushed by connecting a flushing pipeline to the bypass pipe 19.
The preparation method of the reagent for rapidly detecting pantothenic acid in food comprises the following steps:
A. placing concentrated hydrochloric acid stock solution into a volumetric flask, and adding water to dilute the stock solution to 1000mL;
B. taking zinc sulfate heptahydrate, adding water for dissolution and fixing the volume to 100mL;
C. dissolving potassium dihydrogen phosphate in water, adjusting pH to 3.0 with phosphoric acid, diluting to 1000mL with water, and filtering with 0.45 μm filter membrane;
D. taking a D-calcium pantothenate solution, adding water to fix the volume to 1000mL;
E. and (3) removing the sealing plug 6, placing the solution prepared in the steps A-D into the reagent transparent storage tank 5, and then re-covering the sealing plug 6 for later use.
The application of the rapid detection reagent for pantothenic acid in food in detecting pantothenic acid in food comprises the following specific steps of:
A. crushing and uniformly mixing the solid sample; the carbonic acid beverage needs ultrasonic wave to remove carbon dioxide, and other liquid samples are uniformly shaken.
B. For nutrient supplement health-care food, accurately weighing or measuring a proper amount of sample (m) to 0.001g, generally 0.2 g-2 g of solid sample, 10 g-20 g of liquid sample, placing into a 50mL conical flask, adding 30mL warm water at 40-50 ℃ for ultrasonic extraction for 20min, and fixing volume to scale (V) with water. Transferring into a centrifuge tube 3000r/min for centrifugation for 5-10 min, taking supernatant, filtering with a 0.45 μm filter membrane, and measuring the filtrate on a machine.
For formula food, an appropriate amount of sample (m) is accurately weighed to the nearest 0.001g, typically about 5g for solid sample and about 20g for liquid sample. Put into a 100mL conical flask, and warm water with the temperature of 40-50 ℃ is added to 30mL. If the sample contains starch, adding 0.2g of amylase, shaking and mixing uniformly, covering a bottle stopper, and carrying out shaking enzymolysis for 120-240 min under the water bath condition of 55+/-5 ℃. If the sample does not contain starch, the sample is directly subjected to ultrasonic extraction for 20min. The sample solution was taken out, cooled to room temperature, and the pH was adjusted to 5.0.+ -. 0.1 with 0.1mol/L hydrochloric acid, and 5mL of a 0.5mol/L zinc sulfate solution was added thereto, followed by thorough mixing. Transferring into a 50mL volumetric flask, fixing the volume to the scale with water, fully and uniformly mixing, transferring into a centrifuge tube 3000r/min, centrifuging for 5-10 min, taking supernatant, passing through a 0.45 mu m filter membrane, and taking filtrate to be measured by a machine.
If necessary, the sample measurement solution is diluted with water to give a pantothenic acid concentration of 1. Mu.g/mL-32. Mu.g/mL.
Within the range of
C. The conditions of the liquid phase chromatography are that,
chromatography column ODS (C18), (particle size 5 μm,250 mm. Times.4.6 mm)
Column temperature of 28 ℃ +/-0.5 DEG C
Ultraviolet detector with detection wavelength of 210nm
Mobile phase 0.02mol/L potassium dihydrogen phosphate solution+acetonitrile=95+5
Flow rate 1.0mL/mi
The sample injection amount is 10 mu L or 20 mu L;
D. according to established chromatographic conditions, the pantothenic acid standard working solution is subjected to chromatographic analysis in sequence, and the standard peak-out time and chromatographic peak height (or peak area) are recorded. Drawing a standard curve by taking the concentration of the standard working solution as an abscissa and the peak height (or peak area) as an ordinate;
E. taking a sample measuring solution, carrying out chromatographic analysis according to chromatographic conditions, and searching corresponding pantothenic acid concentration (rho) from a standard curve according to the peak height (or peak area) of the sample;
F. the content of pantothenic acid in the sample is calculated by the following formula:
wherein X is pantothenic acid content in the sample, the solid sample unit is milligrams per hundred grams (mg/100 g), and the liquid sample unit is milligrams per hundred milliliters (mg/100 mL); ρ is the concentration of pantothenic acid in the sample assay solution in micrograms per milliliter (μg/mL) from a standard curve; v is the total volume of the sample measurement solution, and the unit is milliliter (mL); f is the dilution of the sample measuring solution; m is the mass of the sample, and the unit is gram (g).
In the description of the present invention, it should be understood that the terms "longitudinal," "transverse," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate description of the present invention, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present invention.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (2)
1. An application of a reagent taking mechanism in detecting pantothenic acid in food is characterized in that the reagent for rapidly detecting pantothenic acid in food,
comprises 0.1mol/L hydrochloric acid, 0.5mol/L zinc sulfate solution, 0.02mol/L potassium dihydrogen phosphate solution, and 1mg/L D-calcium pantothenate solution;
the detection of pantothenic acid in a food comprises the steps of:
A. placing concentrated hydrochloric acid stock solution into a volumetric flask, and adding water to dilute the stock solution to 1000mL;
B. taking zinc sulfate heptahydrate, adding water for dissolution and fixing the volume to 100mL;
C. dissolving potassium dihydrogen phosphate in water, adjusting pH to 3.0 with phosphoric acid, diluting to 1000mL with water, and filtering with 0.45 μm filter membrane;
D. taking a D-calcium pantothenate solution, adding water to fix the volume to 1000mL;
E. b, removing the sealing plug (6), placing the solution prepared in the steps A-D into a reagent transparent storage tank (5), and then re-covering the sealing plug (6) for later use;
the reagent taking mechanism comprises a machine shell (1), a top cover (2) capable of opening and closing is arranged at the top of the machine shell (1), a refrigeration compressor (3) and a refrigeration coil (4) connected with the refrigeration compressor (3) are arranged at the bottom of the machine shell (1), a plurality of reagent transparent storage tanks (5) are arranged at the top of the machine shell (1) in the top cover (2), scale marks are arranged on the surfaces of the reagent transparent storage tanks (5), a detachable sealing plug (6) is arranged at the top of the reagent transparent storage tanks (5), a flexible air pipe (7) is fixed on the sealing plug (6), one end of the flexible air pipe (7) is positioned in the reagent transparent storage tanks (5), the other end of the flexible air pipe (7) is connected with a nitrogen tank (8), and a titration valve (9) is arranged at the bottoms of the side walls of the reagent transparent storage tanks (5);
the titration valve (9) comprises a valve body (10), a valve cavity (11) is arranged in the valve body (10), a liquid inlet hole (12) communicated with the reagent transparent storage tank (5) is formed in the side wall of the valve cavity (11), a liquid outlet hole (13) is formed in the side wall of the valve cavity (11), a dropper (14) is connected to the outer side of the liquid outlet hole (13), a switch valve (15) is respectively arranged at the liquid inlet end of the liquid inlet hole (12) and the liquid outlet end of the liquid outlet hole (13), a partition plate (16) is movably arranged in the valve cavity (11), a sealing ring (17) in sealing contact with the valve cavity (11) is arranged at the edge of the partition plate (16), a fine adjustment screw (18) is arranged on the valve body (10), one end of the fine adjustment screw (18) is connected with the partition plate (16), and the other end of the fine adjustment screw (18) is positioned at the outer side of the valve body (10); the dropper (14) is arranged obliquely downwards; the side wall of the dropper (14) is provided with a bypass pipe (19), and the bypass pipe (19) is provided with a switch valve (15);
when taking the reagent, keep the ooff valve (15) on liquid hole (13) to close, open ooff valve (15) on feed liquor hole (12), then rotatory fine setting screw (18) according to taking the volume, along with the removal of baffle (16), reagent flows into valve body (10) from reagent transparent storage tank (5), then open ooff valve (15) on liquid hole (13), close ooff valve (15) on feed liquor hole (12), rotatory fine setting screw (18) of opposite direction, baffle (16) carry out the propelling movement to reagent, reagent flows from burette (14).
2. Use of the reagent dispensing mechanism of claim 1 for detecting pantothenic acid in a food product, wherein: the detection method is liquid chromatography.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210225695.8A CN114636766B (en) | 2022-03-09 | 2022-03-09 | Application of reagent taking mechanism in detecting food pantothenic acid |
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