CN106706524A - Method of quickly detecting oxygen content in gas by using fibroin membrane - Google Patents
Method of quickly detecting oxygen content in gas by using fibroin membrane Download PDFInfo
- Publication number
- CN106706524A CN106706524A CN201710096736.7A CN201710096736A CN106706524A CN 106706524 A CN106706524 A CN 106706524A CN 201710096736 A CN201710096736 A CN 201710096736A CN 106706524 A CN106706524 A CN 106706524A
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- Prior art keywords
- oxygen
- oxygen content
- fibroin
- gas
- quick detection
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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
- G01N21/17—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
Abstract
The invention relates to a method of detecting the oxygen content and in particular relates to a method of quickly detecting the oxygen content in gas by using a fibroin membrane, and belongs to the optical field. According to the technical scheme provided by the invention, the method specifically comprises the following steps: degumming a silkworm cocoon layer twice and performing primary salt dissolving, performing dialysis by flowing water for 72h, mixing the dialyzed silkworm cocoon layer with hemoglobin, dropwise adding the mixture onto a polycarbonate sheet after film removal, and drying the polycarbonate sheet in an oven to form a film to obtain an oxygen sensor; and after full contact of the oxygen sensor and to-be-detected gas, performing detection by virtue of a fiber optic spectrometer to obtain the oxygen content. By virtue of the characteristic that the hemoglobin carries oxygen, the hemoglobin is fixed to the fibroin to measure the oxygen content in air, and the method is simple and accurate to measure. Moreover, the used materials are biological materials which are green and environmental-friendly, are relatively long in service life, relatively huge in application value and relatively good in prospect.
Description
Technical field
The present invention relates to optical field, and in particular to hemoglobinated fibroin film is entered using reflecting spectrograph
Row reflection measurement, in the method for oxygen content in quick detection gas.
Background technology
Fibroin is the albumen extracted from silk fiber, with non-toxic, nonirritant and with good ventilative
Penetrability and excellent biocompatibility and biodegradability.In biological technical field, fibroin film can be used as immobilization
The carrier of enzyme and prepare biology sensor.
Hemoglobin is present in the red blood cell of blood, and substantial amounts of hemoglobin is produced during erythrocyte maturation, can be with
It is combined with oxygen.The method of prior art detection oxygen content has a lot, mainly there is chemical method, electrochemical process, zirconium oxide concentration difference electricity
Chi Fa, yellow phosphorus luminescence method, coulometry, the analysis of magnetic-type oxygen, gas chromatography and gas chromatography mass spectrometry method etc., conventional method is time-consuming to take
Power, operation inconvenience, and require that external condition is more harsh；Some service lifes do not grow, be difficult to reuse, waste of resource.
The content of the invention
In order to solve the above technical problems, be fixed to hemoglobin in fibroin by the present invention, being prepared for one kind can examine
The fibroin film of oxygen determination Gas content, and determine its reflectance spectrum by reflecting spectrograph, is contained with oxygen in this determination gas
Amount.
Technical scheme is as follows：A kind of method of oxygen content in use fibroin film quick detection gas,
Comprise the following steps：
(1) preparation of oxygen sensor：Degumming twice, a salt solution, and flowing water dialysis 72h are carried out to silk cocoon layer, is obtained
It is the fibroin solutions of 4.1%-4.5% to volumetric concentration, volumetric concentration is then condensed into 6.8%-7.2%, will concentrates
Fibroin solutions afterwards are with hemoglobin with 1:After 50 volume ratio is well mixed, the poly- carbonic acid after demoulding treatment is added drop-wise to
On ester thin slice, drying and forming-film, as oxygen sensor in an oven；The oxygen sensor for preparing be fibroin with it is blood red
The film of protein mixture, fibroin has non-toxic, nonirritant and with good breathable moisture permeability and excellent life
Thing compatibility and biodegradability, in biological technical field, the fibroin membrane prepared with fibroin can be used as immobilised enzymes
Carrier and prepare biology sensor.
(2) detect：Oxygen sensor is placed in the mixed gas of different oxygen concentrations, according to reflected intensity and different oxygen
The relation of Gas content draws standard curve；Oxygen sensor is placed under test gas again, gas to be measured is calculated according to standard curve
Oxygen content in body；
Described standard curve is：Y=0.82907x+27.3115.
Further, 5wt% Carbon Dioxide sodium solutions are used in described scouring processes, 50wt% is used in salt solution preocess
Anhydrous calcium chloride solution.
Further, described usually time twice is 30min.
Further, the described salt solution time is 5min.
Further, described polycarbonate sheet is by following treatment：Ultrasonically treated 2min in methyl alcohol is placed in, then is placed in
Ultrasonically treated 15min, is then dried under nitrogen flowing in ultra-pure water, finally adds perfluoro capryl trichlorosilane to carry out at demoulding
Reason.
Further, oxygen sensor is placed in 0.5 hour under test gas when described step (2) is detected, continues 0.5
Hour is complete in order to ensure the effect of G＆O sensor, reaches balance.
Further, described oxygen sensor thickness is 1-3mm, and its thickness and fibroin and hemoglobin contain
Amount is related, and content is higher, and oxygen sensor is thicker；Thickness between 1-3 mm when, Detection results are best.
Beneficial effects of the present invention are as follows：Hemoglobin is contained within ferroheme, and ferroheme is the porphyrin compound containing iron,
By the effect of oxygen, iron is set to become divalence and trivalent, so as to produce the change of spectrum；Hemoglobin is combined into fibroin
Film, hemoglobin can just preserve its bioactivity without preserving in aqueous in fibroin desciccator diaphragm, can be with reversible
Combination oxygen, without this characteristic if with reference to other albumen, hemoglobin will be denatured the function of losing and carry oxygen；In addition,
Desciccator diaphragm of the invention preserves and carries all very convenient safety.The mixture of different content oxygen and nitrogen, with oxygen content
Raise, reflection spectrum peak rising high.The present invention carries the characteristic of oxygen using hemoglobin, is fixed in fibroin,
Content of oxygen in air is measured, method is easy, determine accurate, and material therefor is all biomaterial, environmental protection,
And service life is more long, its application value is larger, and prospect is preferable.
Brief description of the drawings
Fig. 1 is the spectrogram of the silk solution using ultraviolet spectrometer detection fibroin solutions and containing hemoglobin；
Fig. 2 is the oxygen sensor that the present invention is prepared；
Fig. 3 is the standard curve for detecting gas with various oxygen content；
Fig. 4 is to detect the reflectance spectrum figure that the gas of different oxygen contents is obtained；
Fig. 5 is the reflectance spectrum figure of oxygen content in the detection gas of embodiment 3.
Specific embodiment
Technical scheme is further described with reference to specific embodiment, but the present invention is not with any shape
Formula is limited to embodiment content.Test method described in embodiment unless otherwise specified, is conventional method；Such as without special theory
Bright, the reagent and biomaterial are commercially obtained.
Embodiment 1
Prepare oxygen sensor
(1) the Carbon Dioxide sodium solution 200mL of 5wt% is prepared, is boiled, being put into 6.0g silk cocoons layer carries out first time degumming
30min, the incomplete boiled silk albumen that will be obtained dries 1h at 55 DEG C.
(2) second degumming process completely is carried out according to the method for first time degumming, obtains the fibroin of complete degumming,
55 DEG C of drying 1h are standby.
(3) the anhydrous calcium chloride solution 40ml of 50wt% is prepared, is boiled, be put into the fibroin albumen that dries of complete degumming, it is molten
Solution, boils 5min, the fibroin albumen of complete degumming is become solution.
(4) solution that will be obtained is transferred in bag filter, and flowing water dialysis 72h, the fibroin solutions that will finally obtain enter
Row concentration, obtains the fibroin solutions that volumetric concentration is 7.0%, this fibroin solutions is detected, curve in such as Fig. 1
a。
(5) by the fibroin solutions after concentration and hemoglobin with 1:After 50 volume ratio is well mixed, this mixed liquor
Detected such as curve b in Fig. 1, mixed liquor is added drop-wise in the polycarbonate sheet after demoulding treatment, be dried in an oven
Film, as oxygen sensor, it is as shown in Figure 2 that thickness is about 2mm.
Embodiment 2
Draw standard curve
(1) oxygen sensor is respectively placed in the nitrogen oxygen atmosphere that oxygen content is 10%, 20%, 30%, 40%, 50%
In body, taken out after 0.5h, by using USB4000 fiber spectrometers, obtain the relation of reflected intensity and oxygen content, standard curve
Such as Fig. 3, spectrogram is shown in Fig. 4.
Embodiment 3
Air to be detected is passed through and is placed with the confined space of oxygen sensor prepared by embodiment 1, be continually fed into
0.5 hour, detected by with USB4000 fiber spectrometers, detection figure according to standard curve as shown in figure 5, calculate gas
The content of middle oxygen, result of calculation is：21.3%, (oxygen content 21.7% in actual air) illustrates present invention detection oxygen
Method error it is small, as a result accurately.
Claims (7)
1. in a kind of use fibroin film quick detection gas oxygen content method, it is characterised in that comprise the following steps：
(1) preparation of oxygen sensor：Degumming twice, a salt solution, and flowing water dialysis 72h are carried out to silk cocoon layer, body is obtained
Product concentration is the fibroin solutions of 4.1%-4.5%, volumetric concentration then is condensed into 6.8%-7.2%, after concentration
Fibroin solutions are with hemoglobin with 1:After 50 volume ratio is well mixed, the makrolon being added drop-wise to after demoulding treatment is thin
On piece, drying and forming-film, as oxygen sensor in an oven；
(2) detect：Oxygen sensor is placed in the mixed gas of different oxygen concentrations, is contained according to reflected intensity and different oxygen
The relation of amount draws standard curve；Oxygen sensor is placed under test gas again, according in standard curve calculating under test gas
Oxygen content；
Described standard curve is：Y=0.82907x+27.3115.
2. as claimed in claim 1 using the method for oxygen content in fibroin film quick detection gas, it is characterised in that
5wt% Carbon Dioxide sodium solutions are used in described scouring processes, 50wt% anhydrous calcium chloride solution is used in salt solution preocess.
3. as claimed in claim 1 using the method for oxygen content in fibroin film quick detection gas, it is characterised in that
Described usually time twice is 30min.
4. as claimed in claim 1 using the method for oxygen content in fibroin film quick detection gas, it is characterised in that
The described salt solution time is 5min.
5. as claimed in claim 1 using the method for oxygen content in fibroin film quick detection gas, it is characterised in that
Described polycarbonate sheet is by following treatment：Ultrasonically treated 2min in methyl alcohol is placed in, then is placed in ultrasonically treated in ultra-pure water
15min, is then dried under nitrogen flowing, finally adds perfluoro capryl trichlorosilane to carry out demoulding treatment.
6. as claimed in claim 1 using the method for oxygen content in fibroin film quick detection gas, it is characterised in that
Be placed in oxygen sensor 0.5 hour under test gas when detecting by described step (2).
7. as claimed in claim 1 using the method for oxygen content in fibroin film quick detection gas, it is characterised in that
Described oxygen sensor thickness is 1-3mm.
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| CN201710096736.7A CN106706524B (en) | 2017-02-22 | 2017-02-22 | A method of using oxygen content in the quick detection gas of fibroin film |
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| CN201710096736.7A CN106706524B (en) | 2017-02-22 | 2017-02-22 | A method of using oxygen content in the quick detection gas of fibroin film |
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| CN106706524B CN106706524B (en) | 2019-04-19 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107132220A (en) * | 2017-06-20 | 2017-09-05 | 大连大学 | A kind of portable oxygen content high speed detector |
| CN111982840A (en) * | 2020-07-31 | 2020-11-24 | 大连大学 | Fibroin one-dimensional photonic crystal sensor for rapidly detecting humidity in environment |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1635370A (en) * | 2003-12-30 | 2005-07-06 | 中国科学院兰州化学物理研究所 | Method for preparing biosensor |
| JP2006117612A (en) * | 2004-10-25 | 2006-05-11 | Ichimaru Pharcos Co Ltd | Active oxygen eliminating agent |
| CN101721751A (en) * | 2008-10-10 | 2010-06-09 | 张阳德 | Human tissue engineering support loaded with controlled-release cell growth factor and provided with hollow silicon dioxide ball with kernel and preparation method and applications thereof |
| CN103923965A (en) * | 2014-05-11 | 2014-07-16 | 徐华 | Fibroin micro-molecule polypeptide preparing method |
| US20140335159A1 (en) * | 2010-04-20 | 2014-11-13 | Vindico NanoBio Technology Inc. | Biodegradable Nanoparticles as Novel Hemoglobin-Based Oxygen Carriers and Methods of Using the Same |
-
2017
- 2017-02-22 CN CN201710096736.7A patent/CN106706524B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1635370A (en) * | 2003-12-30 | 2005-07-06 | 中国科学院兰州化学物理研究所 | Method for preparing biosensor |
| JP2006117612A (en) * | 2004-10-25 | 2006-05-11 | Ichimaru Pharcos Co Ltd | Active oxygen eliminating agent |
| CN101721751A (en) * | 2008-10-10 | 2010-06-09 | 张阳德 | Human tissue engineering support loaded with controlled-release cell growth factor and provided with hollow silicon dioxide ball with kernel and preparation method and applications thereof |
| US20140335159A1 (en) * | 2010-04-20 | 2014-11-13 | Vindico NanoBio Technology Inc. | Biodegradable Nanoparticles as Novel Hemoglobin-Based Oxygen Carriers and Methods of Using the Same |
| CN103923965A (en) * | 2014-05-11 | 2014-07-16 | 徐华 | Fibroin micro-molecule polypeptide preparing method |
Non-Patent Citations (1)
| Title |
|---|
| 陶俊逸等: "蚕丝蛋白制备方法的研究", 《蚕桑通报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107132220A (en) * | 2017-06-20 | 2017-09-05 | 大连大学 | A kind of portable oxygen content high speed detector |
| CN111982840A (en) * | 2020-07-31 | 2020-11-24 | 大连大学 | Fibroin one-dimensional photonic crystal sensor for rapidly detecting humidity in environment |
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| CN106706524B (en) | 2019-04-19 |
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