CN113008784A - Optical fiber device and method for detecting reducing sugar - Google Patents
Optical fiber device and method for detecting reducing sugar Download PDFInfo
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- CN113008784A CN113008784A CN201911319695.9A CN201911319695A CN113008784A CN 113008784 A CN113008784 A CN 113008784A CN 201911319695 A CN201911319695 A CN 201911319695A CN 113008784 A CN113008784 A CN 113008784A
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- 235000000346 sugar Nutrition 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 102
- 238000002156 mixing Methods 0.000 claims abstract description 61
- 239000007788 liquid Substances 0.000 claims abstract description 59
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 39
- 238000001228 spectrum Methods 0.000 claims abstract description 22
- 230000003287 optical effect Effects 0.000 claims abstract description 19
- 238000001514 detection method Methods 0.000 claims abstract description 12
- 150000008163 sugars Chemical class 0.000 claims abstract description 7
- 238000004401 flow injection analysis Methods 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000002347 injection Methods 0.000 claims description 14
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- 239000012295 chemical reaction liquid Substances 0.000 claims description 5
- 239000000835 fiber Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000002699 waste material Substances 0.000 claims description 5
- LWFUFLREGJMOIZ-UHFFFAOYSA-N 3,5-dinitrosalicylic acid Chemical compound OC(=O)C1=CC([N+]([O-])=O)=CC([N+]([O-])=O)=C1O LWFUFLREGJMOIZ-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000002120 nanofilm Substances 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 235000010265 sodium sulphite Nutrition 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- RSJOBNMOMQFPKQ-UHFFFAOYSA-L copper;2,3-dihydroxybutanedioate Chemical compound [Cu+2].[O-]C(=O)C(O)C(O)C([O-])=O RSJOBNMOMQFPKQ-UHFFFAOYSA-L 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- CEQFOVLGLXCDCX-WUKNDPDISA-N methyl red Chemical compound C1=CC(N(C)C)=CC=C1\N=N\C1=CC=CC=C1C(O)=O CEQFOVLGLXCDCX-WUKNDPDISA-N 0.000 claims description 2
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000276 potassium ferrocyanide Substances 0.000 claims description 2
- 239000012286 potassium permanganate Substances 0.000 claims description 2
- 230000008054 signal transmission Effects 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 239000001476 sodium potassium tartrate Substances 0.000 claims 1
- 239000000523 sample Substances 0.000 description 77
- 235000013305 food Nutrition 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
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- 229940074439 potassium sodium tartrate Drugs 0.000 description 3
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- 240000009088 Fragaria x ananassa Species 0.000 description 1
- 235000011363 Fragaria x ananassa Nutrition 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
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- 238000010364 biochemical engineering Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000013586 microbial product Substances 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 235000012015 potatoes Nutrition 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229940001482 sodium sulfite Drugs 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/39—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using tunable lasers
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- Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Optics & Photonics (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses an optical fiber device for detecting reducing sugar, which comprises a sample mixing reaction tank, a reflecting mirror surface, an optical fiber/optical fiber bundle, an optical fiber laser and a spectrum analyzer; the sample mixing reaction pool is provided with a sample inlet of a liquid to be detected and a sample inlet of a reaction reagent; a temperature control device is arranged in the sample mixing reaction tank; the reflecting mirror is arranged in the sample mixing reaction tank; one end of the optical fiber/optical fiber bundle vertically faces the reflecting mirror surface, and the other end of the optical fiber/optical fiber bundle is respectively connected with the optical fiber laser and the optical spectrum analyzer through the coupler; a gap is formed between one end of the optical fiber/optical fiber bundle, which vertically faces the reflector surface, and the gap is not more than 0.02 mm. And methods for detecting reducing sugars are disclosed. The invention makes the input signal and the output signal pass through the same optical fiber/optical fiber bundle through the vertical reflection mode, and avoids the step of removing bubbles in the testing process by controlling the distance between the end surface of the optical fiber/optical fiber bundle and the reflector surface, thus being suitable for popularization and application in the detection of reducing sugar.
Description
Technical Field
The invention relates to the technical field of analysis sensing, in particular to an optical fiber device and method for detecting reducing sugar.
Background
The content of reducing sugar has great influence on the form, the tissue structure, the physicochemical property, the color, the fragrance, the taste and the like of the food, is an important mark of high and low nutritional value of the food, and is an important index of the food quality. If the content of reducing sugar in the edible product is higher, the product may absorb moisture, become soft, go out of water, and deteriorate due to poor storage stability; if the content of reducing sugar is low, small crystal blocks may be formed and hardened before the edible product is shaped, the flavor and quality of the edible product are affected, and the fermentation process and the yield of the edible product are affected. The proportion of reducing sugar to non-reducing sugar in the food can be known through the content of the reducing sugar, and a basis is provided for the modulation improvement of food flavor and the identification of the authenticity and the quality of the food. Therefore, the determination of the content of the reducing sugar has important significance and practical value in the fields of microbial fermentation, biological pharmacy, biochemical engineering, starch sugar products, food and beverage, various health care products and the like.
Researchers have designed many different devices to measure the content of reducing sugar in substances, including ultraviolet-visible spectrophotometer, high performance liquid chromatograph, ion chromatograph, atomic absorption spectrometer, etc., but all have some disadvantages. For example, the ultraviolet-visible spectrophotometer method has expensive instruments and equipment, complicated operation steps, large amount of required standard substances, great influence by external conditions, and is not beneficial to industrial application and detection of a large amount of samples; the high performance liquid chromatograph needs to use a refractive index difference detector, has quite strict requirements on environment and poor repeatability, and has the defects of expensive instrument and equipment, low sensitivity, long system balance time, large quantity of required standard products, great influence of external conditions and the like; atomic absorption spectrometers also suffer from the disadvantages of expensive equipment and cumbersome operation. Moreover, the above methods for measuring the content of reducing sugar are all performed by using a transmission mode, and the method for measuring reducing sugar in the transmission mode is difficult to avoid the influence of bubbles in the solution. Therefore, it is necessary to explore new ways to detect reducing sugars.
Disclosure of Invention
In view of the above, the present invention provides an optical fiber apparatus and method for detecting reducing sugar, which enable an input signal and an output signal to pass through the same optical fiber/optical fiber bundle in a vertical reflection mode, thereby simplifying a complicated design of a transmission mode.
In order to achieve the purpose, the invention adopts the following technical scheme:
an optical fiber device for detecting reducing sugar comprises a sample mixing reaction tank, a reflecting mirror surface, an optical fiber/optical fiber bundle, an optical fiber laser and a spectrum analyzer;
the sample mixing reaction pool is provided with a sample inlet of a liquid to be detected and a sample inlet of a reaction reagent; a temperature control device is arranged in the sample mixing reaction tank;
the reflecting mirror is arranged in the sample mixing reaction tank;
one end of the optical fiber/optical fiber bundle vertically faces the reflecting mirror surface, and the other end of the optical fiber/optical fiber bundle is respectively connected with the optical fiber laser and the optical spectrum analyzer through the coupler;
a gap is formed between one end of the optical fiber/optical fiber bundle, which vertically faces the reflector surface, and the gap is not more than 0.02 mm.
The temperature control device is used for adjusting the temperature of the mixed liquid of the liquid to be detected and the reaction reagent, so that reducing sugar in the liquid to be detected reacts, and detection can be carried out after the reaction is finished. One end of the optical fiber/optical fiber bundle vertically faces the reflecting mirror surface, a certain gap is reserved between the optical fiber/optical fiber bundle and the mirror surface, after the optical fiber laser outputs an optical signal, the light is transmitted out from one end of the optical fiber/optical fiber bundle, is transmitted to the reflecting mirror surface through reaction liquid at the gap, and is transmitted back to the optical fiber/optical fiber bundle through the reaction liquid after being vertically reflected. The device design is simple, and convenient operation is suitable for popularization and application in the detection of reducing sugar.
Preferably, a stirring device is arranged in the sample mixing reaction tank, so that the liquid to be detected and the reaction reagent can be promoted to be fully mixed, and the reaction is quicker and more full.
Preferably, the stirring device is a magnetic stirrer.
Preferably, the optical fiber device for detecting reducing sugar further comprises a first flow injection pump and a second flow injection pump;
the first flow injection pump is used for pumping the liquid to be detected into the sample mixing reaction tank from the liquid sample inlet to be detected;
and the second flow injection pump is used for pumping the reaction reagent into the sample mixing reaction tank from the reaction reagent injection port.
The arrangement of the flow injection pump enables the detection process to be highly automated, and the accuracy of sample introduction is ensured.
Preferably, the temperature control means includes a thermostatic control means with a temperature sensor, and performs temperature adjustment according to a preset temperature while detecting the temperature of the mixed liquid in the sample mixing reaction chamber.
Preferably, the sample mixing reaction cell is provided with a waste liquid discharge port.
A method for detecting reducing sugar adopts a direct vertical reflection mode of an optical fiber/optical fiber bundle, so that incident light and reflected light transmit and feed back information through the same optical fiber/optical fiber bundle channel; reacting the solution to be detected with a reaction reagent to obtain a reaction solution, wherein an optical signal transmission path passes through the reaction solution; and judging the content of reducing sugar in the liquid to be detected according to the intensity, the shade, the optical density, the resonance wavelength or the phase of the reflected light.
Preferably, the detection is performed by using the device, which comprises the following steps:
(1) cleaning a sample mixing reaction tank and a pipeline channel for sample introduction;
(2) respectively introducing a solution to be detected and a reaction reagent into a sample mixing reaction tank through a solution sample inlet and a reaction reagent sample inlet to be detected and fully mixing;
(3) adjusting the temperature through a temperature control device to enable the liquid to be detected to react with the reaction reagent;
(4) the optical signal sent by the fiber laser is transmitted out through the optical fiber/optical fiber bundle, is vertically reflected by the reflecting mirror surface and then is transmitted back to the optical fiber/optical fiber bundle, and the feedback signal is received by the spectrum analyzer;
(5) according to the reflected light intensity, the color depth, the optical density, the resonance wavelength or the phase information received by the spectrum analyzer, comparing with a linear curve of the standard liquid, and analyzing the content of reducing sugar in the liquid to be detected;
(6) removing the reaction liquid from the sample mixing reaction tank after detection;
(7) fully washing a sample mixing reaction tank and a pipeline channel for sample introduction by using deionized water;
(8) and (5) testing the next sample according to the steps (2) to (5).
Preferably, the reaction reagent is a reagent capable of reacting with reducing sugar, and comprises 2 or more than 2 of sodium hydroxide, copper sulfate, methylene blue, concentrated sulfuric acid, crystalline phenol, potassium permanganate, potassium ferrocyanide, 3, 5-dinitrosalicylic acid, glycerol, ferric sulfate, hydrochloric acid, methyl red, ethanol, copper tartrate, potassium sodium tartrate and sodium sulfite.
Preferably, the material of the reflecting mirror surface includes one or more of gold, silver, aluminum, titanium dioxide, zirconium dioxide and platinum, and is used for reflecting the optical signal.
Preferably, the surface of the reflecting mirror surface is plated with a polymer transparent nano film with the thickness of 10nm-100 μm, so that the possible corrosion of chemical reaction on the reflecting mirror surface can be effectively avoided, and the accuracy of a measuring result is further ensured.
According to the technical scheme, the direct vertical reflection mode is adopted, so that the input signal and the output signal pass through the same optical fiber or the same optical fiber bundle, the complex design of the transmission mode is simplified, and the manufacturing cost of the device is effectively reduced. By controlling the distance between the end face of the optical fiber or the optical fiber bundle and the reflector surface, the step that air bubbles need to be removed in the testing process is avoided, reducing sugar can be measured in real time without cooling and removing the air bubbles, the assembly procedure is simplified, the detection time is shortened, and the method has wide commercial application prospects in the fields of food safety, industrial fermentation, microbial product analysis and the like.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention;
in the figure: 1. the device comprises a fiber laser, 2, a coupler, 3, a fiber bundle, 4, a first flow injection pump, 5, a second flow injection pump, 6, a liquid sample inlet to be detected, 7, a reaction reagent sample inlet, 8, a sample mixing reaction tank, 9, a reflector, 10, a waste liquid discharge port, 11, a magnetic stirrer, 12, a temperature control device, 13, a spectrum analyzer, 14 and a computer.
FIG. 2 is a linear plot of reducing sugar concentration versus resonant wavelength.
FIG. 3 is a linear plot of reducing sugar concentration versus normalized color value.
FIG. 4 is a linear plot of reducing sugar concentration versus light intensity signal.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
As shown in FIG. 1, an optical fiber device for detecting reducing sugar comprises a sample mixing reaction tank 8, a reflecting mirror surface 9, an optical fiber bundle 3, an optical fiber laser 1 and an optical spectrum analyzer 13.
The top of the sample mixing reaction pool 8 is provided with a sample inlet 6 of the liquid to be detected and a sample inlet 7 of the reaction reagent, and the bottom of one side is provided with a waste liquid discharge port 10 (provided with a valve or a plug);
a first flow injection pump 4 pumps a liquid to be detected into a sample mixing reaction tank 8 from a liquid to be detected sample inlet 6;
the second flow injection pump 5 pumps the reaction reagent into the sample mixing reaction tank 8 from the reaction reagent injection port 7.
A magnetic stirrer 11 and a temperature control device 12 are arranged in the sample mixing reaction tank 8; the temperature control device 12 can be connected to the computer 14, and the computer 14 issues a temperature control command.
The reflector 9 is made of platinum with the thickness of 1mm, and the surface of the reflector is plated with a polytetrafluoroethylene polymer transparent nano film with the thickness of 100 nm; the reflecting mirror 9 is embedded on one side wall of the sample mixing reaction cell 8.
The optical fiber bundle 3 is composed of 50 optical fibers; one end of the reflector is vertically opposite to the reflector 9, and a gap of 0.01mm is formed between the reflector and the reflector 9; the other ends are respectively connected with the fiber laser 1 and the spectrum analyzer 13 through the coupler 2.
The spectrum analyzer 13 may be connected to the computer 14, and the computer 14 may be used to analyze the feedback information.
The detection is carried out by using the device, and the method comprises the following steps:
(1) cleaning a sample mixing reaction pool 8 and a pipeline channel for sample injection (including a pipeline between a first flow injection pump 4 and a sample injection port 6 of a liquid to be detected and a pipeline between a second flow injection pump 5 and a reaction reagent sample injection port 7);
(2) respectively introducing a liquid to be detected and a reaction reagent into a sample mixing reaction tank 8 through a liquid to be detected injection port 6 and a reaction reagent injection port 7 by using a first flow injection pump 4 and a second flow injection pump 5; under the action of the magnetic stirrer 11, the liquid to be detected and the reaction reagent are fully mixed;
(3) the temperature is adjusted by a temperature control device 12, so that the liquid to be detected reacts with the reaction reagent;
(4) an optical signal sent by the optical fiber laser 1 is transmitted out through the optical fiber bundle 3, is vertically reflected by the reflecting mirror 9 and then is transmitted back to the optical fiber bundle 3, and a spectrum analyzer 13 receives a feedback signal;
(5) analyzing the content of reducing sugar in the liquid to be detected according to the information received by the spectrum analyzer 13;
(6) after the detection is finished, the reaction liquid is removed from the sample mixing reaction tank 8 through a waste liquid discharge port 10;
(7) the sample mixing reaction tank 8 and a pipeline channel for sample introduction are fully washed by deionized water through the driving of the first flow injection pump 4 and the second flow injection pump 5;
(8) and (5) testing the next sample according to the steps (2) to (5).
Example 2
The reducing sugar sample liquid extracted from wheat flour was measured using the apparatus of example 1:
(1) sequentially washing the sample mixing reaction tank 8 and a pipeline channel for sample injection by using acetone, ethanol and water;
(2) under the action of a first flow injection pump 4, 5ml of reducing sugar sample liquid is injected into a sample mixing reaction tank 8 through a sample inlet 6 of a liquid to be detected; under the action of a second flow injection pump 5, 2.5ml of reaction reagent containing 0.27M of copper sulfate pentahydrate, 2.5 mu L of concentrated sulfuric acid, 1.23M of potassium sodium tartrate and 2.5M of sodium hydroxide is injected into a sample mixing reaction tank 8 through a reaction reagent injection port 7; under the action of a magnetic stirrer 11, fully mixing reducing sugar sample liquid and a reaction reagent in a sample mixing reaction tank 8;
(3) the temperature of the mixed liquid in the sample mixing reaction tank 8 is adjusted by controlling the temperature control device 12 through the computer 14, so that the temperature of the mixed liquid in the sample mixing reaction tank 8 reaches 100 ℃, the substances in the mixed liquid react, and the reaction is finished after the mixed liquid is kept for 5min under the condition of boiling at 100 ℃;
(4) after the reaction is finished, the optical signal sent by the optical fiber laser 1 is transmitted out through the optical fiber bundle 3, vertically reflected by the reflecting mirror 9 and then transmitted back to the optical fiber bundle 3, and the spectrum analyzer 13 receives the feedback resonance wavelength signal;
(5) the data is processed by the computer 14: the content of reducing sugar was estimated to be 22.8% by comparing the resonance wavelength of the feedback received by the spectrum analyzer 13 with 587.33nm, which is the linear curve of the standard sample (FIG. 2, obtained by detecting the standard solutions of reducing sugar at different concentrations as the sample according to the above-mentioned method).
Example 3
The reducing sugar sample solution extracted from potatoes was measured using the apparatus of example 1:
(1) sequentially washing the sample mixing reaction tank 8 and a pipeline channel for sample injection by using acetone, ethanol and water;
(2) under the action of a first flow injection pump 4, 5ml of reducing sugar sample liquid is injected into a sample mixing reaction tank 8 through a sample inlet 6 of a liquid to be detected; under the action of a second flow injection pump 5, 5ml of reaction reagent containing 0.028M of 3, 5-dinitrosalicylic acid, 0.650M of sodium hydroxide and 75 mu L of glycerol is injected into a sample mixing reaction tank 8 through a reaction reagent injection port 7; under the action of a magnetic stirrer 11, fully mixing reducing sugar sample liquid and a reaction reagent in a sample mixing reaction tank 8;
(3) the temperature of the mixed liquid in the sample mixing reaction tank 8 is adjusted by controlling the temperature control device 12 through the computer 14, so that the temperature of the mixed liquid reaches 100 ℃, substances in the mixed liquid react, and the mixed liquid is kept for 10min under the condition of boiling at 100 ℃;
(4) an optical signal sent by the optical fiber laser 1 is transmitted out through the optical fiber bundle 3, is vertically reflected by the reflecting mirror 9 and then is transmitted back to the optical fiber bundle 3, and a spectrum analyzer 13 receives a feedback signal;
(5) the computer 14 is used for processing the light color shade data: the spectrum analyzer 13 received the feedback normalized color value of 0.1601, and compared with the linear curve of the standard sample (fig. 3, obtained by testing the standard solutions of reducing sugars of different concentrations as samples according to the above method), it estimated that the reducing sugar content was 12.8%.
Example 4
The reducing sugar sample solution extracted from strawberry was measured using the apparatus of example 1:
(1) sequentially washing the sample mixing reaction tank 8 and a pipeline channel for sample injection by using acetone, ethanol and water;
(2) under the action of a first flow injection pump 4, 5ml of reducing sugar sample liquid is injected into a sample mixing reaction tank 8 through a sample inlet 6 of a liquid to be detected; under the action of a second flow injection pump 5, 10ml of a reaction reagent containing 0.0276M 3, 5-dinitrosalicylic acid, 0.524M sodium hydroxide, 0.655M potassium sodium tartrate, 0.0531M crystalline phenol and 0.0396M sodium sulfite is injected into a sample mixing reaction tank 8 through a reaction reagent injection port 7; under the action of a magnetic stirrer 11, fully mixing reducing sugar sample liquid and a reaction reagent in a sample mixing reaction tank 8;
(3) the temperature of the mixed liquid in the sample mixing reaction tank 8 is adjusted by controlling the temperature control device 12 through the computer 14, so that the temperature of the mixed liquid reaches 100 ℃, substances in the mixed liquid react, and the mixed liquid is kept for 6min under the condition of boiling at 100 ℃;
(4) an optical signal sent by the optical fiber laser 1 is transmitted out through the optical fiber bundle 3, is vertically reflected by the reflecting mirror 9 and then is transmitted back to the optical fiber bundle 3, and the feedback information is received by the spectrum analyzer 13;
(5) the light intensity signal data is processed by the computer 14: the content of reducing sugar was estimated to be 5.86% by comparing the feedback light intensity signal received by the spectrum analyzer 13 with a linear curve of a standard sample (fig. 4, obtained by detecting a standard solution of reducing sugar at different concentrations as a sample according to the above method).
The general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. An optical fiber device for detecting reducing sugar is characterized by comprising a sample mixing reaction tank, a reflecting mirror surface, an optical fiber/optical fiber bundle, an optical fiber laser and an optical spectrum analyzer;
the sample mixing reaction tank is provided with a sample inlet of a liquid to be detected and a sample inlet of a reaction reagent; a temperature control device is arranged in the sample mixing reaction tank;
the reflecting mirror surface is arranged in the sample mixing reaction pool;
one end of the optical fiber/optical fiber bundle vertically faces the reflecting mirror surface, and the other end of the optical fiber/optical fiber bundle is respectively connected with the optical fiber laser and the spectrum analyzer through a coupler;
and a gap is formed between one end of the optical fiber/optical fiber bundle, which vertically faces the reflector surface, and the gap is not more than 0.02 mm.
2. The optical fiber device for detecting reducing sugar according to claim 1, wherein a stirring device is installed in the sample mixing reaction chamber.
3. The optical fiber apparatus for detecting reducing sugar according to claim 1, further comprising a first flow syringe pump and a second flow syringe pump;
the first flow injection pump is used for pumping the liquid to be detected into the sample mixing reaction tank from the liquid sample inlet to be detected;
the second flow injection pump is used for pumping a reaction reagent into the sample mixing reaction tank from the reaction reagent injection port.
4. The optical fiber device for detecting reducing sugar according to claim 1, wherein the temperature control means comprises a thermostat control means with a temperature sensor.
5. The optical fiber device for detecting reducing sugar according to claim 1, wherein the sample mixing reaction tank is provided with a waste liquid discharge port.
6. A method for detecting reducing sugar is characterized in that an optical fiber/optical fiber bundle direct vertical reflection mode is adopted, so that incident light and reflected light are transmitted and fed back information through the same optical fiber/optical fiber bundle channel; reacting the solution to be detected with a reaction reagent to obtain a reaction solution, wherein an optical signal transmission path passes through the reaction solution; and judging the content of reducing sugar in the liquid to be detected according to the intensity, the shade, the optical density, the resonance wavelength or the phase of the reflected light.
7. The method for detecting reducing sugars according to claim 6, characterized in that the detection is carried out using the device of any one of claims 1 to 5, comprising the following steps:
(1) cleaning a sample mixing reaction tank and a pipeline channel for sample introduction;
(2) respectively introducing a solution to be detected and a reaction reagent into a sample mixing reaction tank through a solution sample inlet and a reaction reagent sample inlet to be detected and fully mixing;
(3) adjusting the temperature through a temperature control device to enable the liquid to be detected to react with the reaction reagent;
(4) the optical signal sent by the fiber laser is transmitted out through the optical fiber/optical fiber bundle, is vertically reflected by the reflecting mirror surface and then is transmitted back to the optical fiber/optical fiber bundle, and the feedback signal is received by the spectrum analyzer;
(5) according to the reflected light intensity, the color depth, the optical density, the resonance wavelength or the phase information received by the spectrum analyzer, comparing with a linear curve of the standard liquid, and analyzing the content of reducing sugar in the liquid to be detected;
(6) removing the reaction liquid from the sample mixing reaction tank after detection;
(7) fully washing a sample mixing reaction tank and a pipeline channel for sample introduction by using deionized water;
(8) and (5) testing the next sample according to the steps (2) to (5).
8. The method for detecting reducing sugars according to claim 6,
the reaction reagent is a reagent capable of reacting with reducing sugar, and comprises 2 or more than 2 of sodium hydroxide, copper sulfate, methylene blue, concentrated sulfuric acid, crystallized phenol, potassium permanganate, potassium ferrocyanide, 3, 5-dinitrosalicylic acid, glycerol, ferric sulfate, hydrochloric acid, methyl red, ethanol, copper tartrate, sodium potassium tartrate and sodium sulfite.
9. The method for detecting reducing sugars according to claim 6,
the reflecting mirror surface is made of one or more of gold, silver, aluminum, titanium dioxide, zirconium dioxide and platinum and is used for reflecting optical signals.
10. The method for detecting reducing sugars according to claim 9,
the surface of the reflecting mirror surface is plated with a high-molecular transparent nano film.
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| CN212586228U (en) * | 2019-12-19 | 2021-02-23 | 山东省科学院生物研究所 | Optical fiber device for detecting reducing sugar |
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| US20030086823A1 (en) * | 2001-11-07 | 2003-05-08 | Fernando C J Anthony | Fiber-optic dissolution systems, devices, and methods |
| CN101750403A (en) * | 2008-12-17 | 2010-06-23 | 中国科学院大连化学物理研究所 | Fluorescent optical fiber sensor for detecting nitrogen dioxide |
| CN205333518U (en) * | 2016-01-13 | 2016-06-22 | 华南理工大学 | Making wine zymotic fluid yeast vigor on -line measuring device based on raman spectroscopy |
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