CN212586228U - Optical fiber device for detecting reducing sugar - Google Patents

Optical fiber device for detecting reducing sugar Download PDF

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Publication number
CN212586228U
CN212586228U CN201922299263.8U CN201922299263U CN212586228U CN 212586228 U CN212586228 U CN 212586228U CN 201922299263 U CN201922299263 U CN 201922299263U CN 212586228 U CN212586228 U CN 212586228U
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optical fiber
sample
reducing sugar
mixing reaction
fiber bundle
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李秋顺
史建国
马耀宏
杨俊慧
蔡雷
杨艳
孟庆军
朱思荣
张显升
李大海
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Biology Institute of Shandong Academy of Sciences
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Biology Institute of Shandong Academy of Sciences
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Abstract

The utility model discloses an optical fiber device for detecting reducing sugar, which comprises a sample mixing reaction tank, a reflector surface, an 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 bundle vertically faces the reflecting mirror surface, and the other end of the 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 bundle, which is vertical to the reflecting mirror surface, and the gap is not more than 0.02 mm. The utility model discloses a vertical reflection mode makes input signal and output signal pass through same fiber bundle, through the distance between control fiber bundle terminal surface and the speculum face, has avoided the test procedure must get rid of the step of bubble, is suitable for popularization and application in the detection of reducing sugar.

Description

Optical fiber device for detecting reducing sugar
Technical Field
The utility model relates to an analysis sensing technical field, more specifically the optical fiber device that relates to a detect reducing sugar that says so.
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.
SUMMERY OF THE UTILITY MODEL
In view of this, the utility model provides an optical fiber device for detecting reducing sugar makes input signal and output signal pass through same fiber bundle through the vertical reflection mode, has simplified the complicated design of transmission mode.
In order to achieve the above purpose, the utility model 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 bundle, an optical fiber laser and an optical 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 bundle vertically faces the reflecting mirror surface, and the other end of the 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 bundle, which is vertical to the reflecting mirror 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 bundle vertically faces the reflecting mirror surface, a certain gap is reserved between the 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 bundle, the reaction liquid is transmitted to the reflecting mirror surface through the gap, and after the vertical reflection, the light is transmitted back to the optical fiber bundle through the reaction liquid. 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.
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 above technical scheme, the utility model discloses a direct vertical reflection mode makes input signal and spread signal pass through same fiber bundle, has simplified the complicated design of transmission mode, has reduced the cost of manufacture of device effectively. By controlling the distance between the end face of 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 prospect in the fields of food safety, industrial fermentation, microbial product analysis and the like.
Drawings
FIG. 1 is a schematic view of the structure of the device 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 described below clearly and completely, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to 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 (including the intensity of reflected light, the shade of color, the optical density, the resonance wavelength or the phase position, and the like) 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).
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.
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 spectrum analyzer 13 receives the feedback at a resonance wavelength of 587.33nm, and calculates the reducing sugar content to be 22.8% by comparing with a linear curve of a standard sample (FIG. 2, obtained by detecting a standard solution of reducing sugar at different concentrations as a sample according to the above 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 (5)

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 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 bundle vertically faces the reflecting mirror surface, and the other end of the 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 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.
CN201922299263.8U 2019-12-19 2019-12-19 Optical fiber device for detecting reducing sugar Active CN212586228U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113008784A (en) * 2019-12-19 2021-06-22 山东省科学院生物研究所 Optical fiber device and method for detecting reducing sugar

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113008784A (en) * 2019-12-19 2021-06-22 山东省科学院生物研究所 Optical fiber device and method for detecting reducing sugar

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