CN109187699A - A method of detection Ancient Silk Textile - Google Patents
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Abstract
The present invention relates to historical relic detection fields, disclose a kind of method for detecting Ancient Silk Textile, the present invention extracts fibroin albumen using formic acid, calcium nitrate solution system, pass through graphene oxide, propane diamine, sodium chloroplatinate later, sodium borohydride mixed system prepares graphene nanometer composite modification working electrode, it modifies Bombyx mori silk fibroin antibody, institute's sample in succession on the working electrode (s, uses Electrochemical Detection current value respectively, whether the variation judgement sample by analyzing current value is silk goods.Method provided by the invention is easy to operate, high sensitivity.
Description
Technical field
The present invention relates to historical relic detection field more particularly to a kind of methods for detecting Ancient Silk Textile.
Background technique
China is exactly textile big country since ancient times, and the textile type of production is abundant, and technique is exquisite, comfortable ventilating.Its
In most well-known textile be exactly China silk, therefore China is otherwise known as " state of silk ".The main component of silk is mulberry
Silk, mulberry silk are mainly made of fibroin albumen and silk gum two parts, and fibroin albumen is the chief component of silk, are accounted for about total
The 70% of weight.And mulberry silk, as a kind of high-molecular organic material, the influence vulnerable to light, heat, soda acid, microorganism etc. occurs
Degradation, so that the variation of the structures such as crystallinity, molecular weight and performance is caused, so conventional detection method sensitivity is low, by miscellaneous
Matter interference effect is big, is not suitable for detecting historical relic, it is therefore desirable to develop that a kind of sensitivity is good, the detection ancient times of high specificity
The method of silk goods.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of methods for detecting Ancient Silk Textile.The present invention uses
Formic acid, calcium nitrate solution system extract fibroin albumen, pass through graphene oxide, propane diamine, sodium chloroplatinate, sodium borohydride later
Mixed system prepares graphene nanometer composite modification working electrode, and modification Bombyx mori silk fibroin is anti-in succession on the working electrode (s
Body, institute's sample use Electrochemical Detection current value respectively, and whether the variation judgement sample by analyzing current value is silk weaving
Product.Method provided by the invention is easy to operate, high sensitivity.
The specific technical proposal of the invention is: a kind of method for detecting Ancient Silk Textile, in terms of g, mg and mL, including it is following
Step:
1) it weighs 4-6g mulberry silk to be placed in sodium carbonate liquor of the 180-220mL containing 0.018-0.022M, water-bath 55-65min, water
Bath temperature is 75-85 DEG C, and taking-up is cleaned more than three times with deionized water, dry.
2) formic acid 48-52mL is added in the fibroin for taking 1.8-2.2g to dry, 2.3-2.7g calcium nitrate, stirs 80-100min,
Filtering addition sodium bicarbonate is in neutrality up to solution, after dialysis freeze-drying, obtained fibroin albumen is pulverized spare, is obtained
To silk fibroin powder.
The present invention dissolves fibroin using calcium nitrate, formic acid system, not only can increase the solubility to fibroin, but also can reduce to silk
The destruction of plain strand, and the dissolution to fibroin can be completed in the system at normal temperature, without heating.
3) it takes 2.8-3.2mL concentration to be immersed in 0.2-0.4M propane diamine for the graphene oxide of 5-7mg/mL to flow back
2.8-3.2h；Then the sodium chloroplatinate of 5-6ml 0.1%(w/v) is added, continuously stirs and in identical temperature reflux 20-
After 40min by 5-7mL 1%w/v sodium borohydride be added dropwise in reaction system, and further return at the same temperature
20-40min is flowed, after cooling down final reflux solution and being centrifuged 9-11min with 5000-6000rpm, 3-5 is washed with deionized
It is secondary.
Graphene nanometer composite prepared by the present invention has a good biocompatibility, biggish specific surface area and good
Absorption property, can not only capture lot of antibodies, electrochemical luminescence signals can also be amplified, improve the sensitivity of detection.
4) 1.8-2.2ml step 3) acquired solution is taken to mix ultrasonic treatment with 5.8-6.2ml n,N-Dimethylformamide
10-20min。
5) electrode 1,2,3 respectively with 0.02 μm of Al2O3After polishing, it is cleaned by ultrasonic with deionized water, with 28-32 μ L step
4) it after acquired solution is added drop-wise to electrode surface, dries in air.
6) by step 5) treated electrode 1,2,3 are placed in the Bombyx mori silk fibroin antibody that 8-12 μ L is diluted to 1000 times
In, it is rinsed after 5-7h is incubated in 1-5 DEG C of environment with 7.4 buffer of PBS, is then incubated for 28- with the BSA solution of 1wt%
32min is rinsed with 7.4 buffer of PBS.
7) fibroin protein powder obtained by step 2 is taken, with 9.6 buffer of CB at the fibroin albumen of 90-110 μ g/mL
Solution；It takes 0.02-0.2g historical relic sample to be dissolved in 9.6 buffer of 100ml CB, is mixed evenly, stand, take supernatant.
8) it takes in step 7) on the silk fibroin protein solution 8-12 μ L electrode 1 that is added dropwise in step 6) that treated, takes step 7)
On middle historical relic sample solution 8-12 μ L is added dropwise in step 6) that treated electrode 2, and 50- is incubated under 37 DEG C of moist environment
70min is rinsed with 7.4 buffer of PBS.
9) gold electrode 3 of step 6) of learning from else's experience processing and the electrode 1,2 of step 8) processing, in 5Mm [Fe (CN)6]3-/4-Solution
Middle carry out Electrochemical Detection, scanning current potential are -0.2-0.6V, amplitude 0.05V；1,3 gained current peak of electrode is occurred
Difference is as control, if difference occurs in 2,3 current peak of electrode, illustrates that historical relic sample contains mulberry silk, on the contrary then explanation does not contain
Mulberry silk.
The present invention extracts fibroin albumen using formic acid, calcium nitrate solution system, later by graphene oxide, propane diamine,
Sodium chloroplatinate, sodium borohydride mixed system prepare graphene nanometer composite modification working electrode, on the working electrode (s in succession
Bombyx mori silk fibroin antibody, institute's sample are modified, uses Electrochemical Detection current value respectively, the variation by analyzing current value is sentenced
Whether disconnected sample is silk goods.Method provided by the invention is easy to operate, high sensitivity.
Preferably, filtering the cellulose dialysis bag that acquired solution is 8000-10000 with molecular cut off in step 2
It dialyses 2-3 days in deionized water, and changes a water every 5-7h, by silk fibroin protein solution vacuum refrigeration 2-3 days.
Preferably, reflux temperature is 65-75 DEG C in step 3).
Preferably, in step 6) and step 8), the preparation method of 7.4 buffer of PBS are as follows: 0.2 g potassium chloride is weighed,
It is straight that 0.27 g potassium dihydrogen phosphate, 8 g sodium chloride and 1.42 g disodium hydrogen phosphates are added to uniform stirring in 800 mL deionized waters
To after being completely dissolved with volumetric flask constant volume to 1000 mL, the pH to 7.4 of solution is adjusted.
Preferably, in step 7) 9.6 solution of CB preparation method are as follows: weigh 1.5 g sodium carbonate and 2.9 g bicarbonates
Sodium is added to uniform stirring in 800 mL deionized waters until with volumetric flask constant volume to 1000 mL after being completely dissolved, and adjusts molten
The pH to 9.6 of liquid.
Preferably, Electrochemical Detection includes three electrodes in step 9), gold electrode is made as working electrode, platinum electrode
For auxiliary electrode, saturated calomel electrode is as reference electrode.
It is compared with the prior art, the beneficial effects of the present invention are:
(1) Bombyx mori silk fibroin extracting method of the present invention dissolves fibroin using calcium nitrate, formic acid system, both can increase to fibroin
Solubility, and the destruction to fibroin strand can be reduced, and the dissolution to fibroin can be completed in the system at normal temperature, is not necessarily to
Heating.
(2) graphene nanometer composite that the present invention synthesizes has excellent because of biggish specific surface area and nano-scale
Enhanced sensitivity and modifiability modify working electrode with it, can reinforce the sensitivity of testing result.
(3) amount of samples of the present invention is few, quickly, accurately, high sensitivity can detect fibroin albumen, detection is dropped
Serious silk fabric cultural relics are solved to have great importance.
Specific embodiment
The present invention will be further described with reference to the examples below.
Embodiment 1:
1) it weighs 5g mulberry silk to be placed in sodium carbonate liquor of the 180mL containing 0.018M, water-bath 55min, bath temperature is 80 DEG C, is taken
It is cleaned three times with deionized water out, is put into oven drying.
2) formic acid 48mL is added in the fibroin for taking 2g to dry, 2.3g calcium nitrate, and with magnetic agitation 80min, carbonic acid is added in filtering
Hydrogen sodium is in neutrality up to solution, and acquired solution is dialysed in deionized water with the cellulose dialysis bag that molecular cut off is 8000
2 days, and change a water every 5h, after silk fibroin protein solution is freeze-dried 2 days in vacuum freeze drier, the silk that will obtain
Fibroin is pulverized spare.
3) it takes 2.8mL concentration to be immersed in 0.2M propane diamine for the graphene oxide of 5mg/mL to flow back at a temperature of 65 DEG C
2.8h;Then, the sodium chloroplatinate of 5ml 0.1%(w/v) is added in previous mixture, is continuously stirred and identical
5mL 1%w/v sodium borohydride is added dropwise in reaction system after temperature reflux 30 minutes, and at the same temperature into
One step flows back 30 minutes, after cooling down final reflux solution and being centrifuged 9 minutes with 5000rpm, is washed with deionized 3 times.
4) take 1.8ml step 3) acquired solution that 5.8ml n,N-Dimethylformamide mixing ultrasonic treatment 15min is added.
5) gold electrode 1,2,3 with 0.02 μm of Al2O3After polishing, it is cleaned by ultrasonic with deionized water, is handled with 28 μ L step 4)
After solution afterwards is added drop-wise to gold electrode surfaces, dry in air.
6) by step 5) treated electrode 1,2,3, which are placed in 8 μ L, is diluted in 1000 times of Bombyx mori silk fibroin antibody,
It is rinsed after being incubated for 5h in 4 DEG C of environment with 7.4 buffer of PBS, then 28min is incubated for 1wt%BSA solution, with PBS 7.4
Buffer rinses.
The wherein preparation of 7.4 buffer of PBS: weighing 0.2 g potassium chloride, 0.27 g potassium dihydrogen phosphate, 8 g sodium chloride and
1.42 g disodium hydrogen phosphates are added to uniform stirring in 800 mL deionized waters until after being completely dissolved extremely with volumetric flask constant volume
1000 mL adjust the pH to 7.4 of solution.
7) take 9.6 buffer of Bombyx mori silk fibroin powder CB that extracts in step 2 at the fibroin of 100 μ g/mL
Protein solution；It takes 0.02g historical relic sample to be dissolved in 9.6 buffer of 100ml CB, is mixed evenly, stand, take supernatant.
The wherein preparation of 9.6 solution of CB: weighing 1.5 g sodium carbonate and 2.9 g sodium bicarbonates be added to 800 mL go from
Uniform stirring in sub- water adjusts the pH to 9.6 of solution until with volumetric flask constant volume to 1000 mL after being completely dissolved.
8) it takes in step 7) on 8 μ L of the silk fibroin protein solution electrode 1 that is added dropwise in step 6) that treated, takes in step 7)
On 8 μ L of historical relic sample solution is added dropwise in step 6) that treated electrode 2, and it is incubated for 50min under 37 DEG C of moist environment, used
7.4 buffer of PBS rinses.
9) electrode 3 of step 6) of learning from else's experience processing and the electrode 1,2 of step 8) processing, in 5Mm [Fe (CN)6]3-/4-In solution
Electrochemical Detection is carried out, scanning current potential is -0.2-0.6V, and amplitude 0.05V, gold electrode is as working electrode, platinum electrode conduct
Auxiliary electrode, saturated calomel electrode is as reference electrode；The difference that 1,3 gained current peak of electrode is occurred is as control, such as
There is difference in 2,3 current peak of fruit electrode, illustrates that historical relic sample contains mulberry silk, on the contrary then explanation does not have.
Embodiment 2:
1) it weighs 5g mulberry silk to be placed in sodium carbonate liquor of the 200mL containing 0.02M, water-bath 60min, bath temperature is 80 DEG C, is taken
It is cleaned four times with deionized water out, is put into oven drying.
2) formic acid 50mL is added in the fibroin for taking 2g to dry, 2.5g calcium nitrate, and with magnetic agitation 90min, carbonic acid is added in filtering
Hydrogen sodium is in neutrality up to solution, and acquired solution is dialysed in deionized water with the cellulose dialysis bag that molecular cut off is 9000
2.5 days, and a water is changed every 6h, after silk fibroin protein solution is freeze-dried 2.5 days in vacuum freeze drier, it will obtain
Fibroin albumen pulverize it is spare.
3) taking 3mL concentration is that the graphene oxide of 6mg/mL is immersed in 0.3M propane diamine the 3h that flows back at a temperature of 70 DEG C;
Then, the sodium chloroplatinate of 5.5ml 0.1%(w/v) is added in previous mixture, is continuously stirred and mutually synthermal
6mL 1%w/v sodium borohydride is added dropwise in reaction system by reflux after 30 minutes, and at the same temperature further
Reflux 30 minutes, cooling final reflux solution are simultaneously centrifuged after ten minutes with 5500rpm, are washed with deionized 4 times.
4) take 2ml step 3) acquired solution that 6ml n,N-Dimethylformamide mixing ultrasonic treatment 15min is added.
5) gold electrode 1,2,3 with 0.02 μm of Al2O3After polishing, it is cleaned by ultrasonic with deionized water, is handled with 30 μ L step 4)
After solution afterwards is added drop-wise to gold electrode surfaces, dry in air.
6) by step 5) treated electrode 1,2,3, which are placed in 10 μ L, is diluted in 1000 times of Bombyx mori silk fibroin antibody,
It is rinsed after being incubated for 6h in 4 DEG C of environment with 7.4 buffer of PBS, then 30min is incubated for 1wt%BSA solution, with PBS 7.4
Buffer rinses.
The wherein preparation of 7.4 buffer of PBS: weighing 0.2 g potassium chloride, 0.27 g potassium dihydrogen phosphate, 8 g sodium chloride and
1.42 g disodium hydrogen phosphates are added to uniform stirring in 800 mL deionized waters until after being completely dissolved extremely with volumetric flask constant volume
1000 mL adjust the pH to 7.4 of solution.
8) take 9.6 buffer of Bombyx mori silk fibroin powder CB that extracts in step 2 at the fibroin of 100 μ g/mL
Protein solution；It takes 0.02-0.2g historical relic sample to be dissolved in 9.6 buffer of 100ml CB, is mixed evenly, stand, take supernatant
Liquid.
The wherein preparation of 9.6 solution of CB: weighing 1.5 g sodium carbonate and 2.9 g sodium bicarbonates be added to 800 mL go from
Uniform stirring in sub- water adjusts the pH to 9.6 of solution until with volumetric flask constant volume to 1000 mL after being completely dissolved.
8) it takes in step 7) on 10 μ L of the silk fibroin protein solution electrode 1 that is added dropwise in step 6) that treated, takes in step 7)
On 10 μ L of historical relic sample solution is added dropwise in step 6) that treated electrode 2, and it is incubated for 60min under 37 DEG C of moist environment, used
7.4 buffer of PBS rinses.
9) electrode 3 of step 6) of learning from else's experience processing and the electrode 1,2 of step 8) processing, in 5Mm [Fe (CN)6]3-/4-In solution
Electrochemical Detection is carried out, scanning current potential is -0.2-0.6V, and amplitude 0.05V, gold electrode is as working electrode, platinum electrode conduct
Auxiliary electrode, saturated calomel electrode is as reference electrode；The difference that 1,3 gained current peak of electrode is occurred is as control, such as
There is difference in 2,3 current peak of fruit electrode, illustrates that historical relic sample contains mulberry silk, on the contrary then explanation does not have.
Embodiment 3:
1) it weighs 5g mulberry silk to be placed in sodium carbonate liquor of the 220mL containing 0.022M, water-bath 65min, bath temperature is 80 DEG C, is taken
It is cleaned five times with deionized water out, is put into oven drying.
2) formic acid 52mL is added in the fibroin for taking 2g to dry, 2.7g calcium nitrate, and with magnetic agitation 100min, carbon is added in filtering
Sour hydrogen sodium until solution be in neutrality, by acquired solution molecular cut off be 10000 cellulose dialysis bag in deionized water
Dialysis 3 days, and a water is changed every 7h, after silk fibroin protein solution is freeze-dried 3 days in vacuum freeze drier, it will obtain
Fibroin albumen pulverize it is spare.
3) it takes 3.2mL concentration to be immersed in 0.4M propane diamine for the graphene oxide of 7mg/mL to flow back at a temperature of 75 DEG C
3.2h;Then, the sodium chloroplatinate of 6ml 0.1%(w/v) is added in previous mixture, is continuously stirred and identical
7mL 1%w/v sodium borohydride is added dropwise in reaction system after temperature reflux 30 minutes, and at the same temperature into
One step flows back 30 minutes, after cooling down final reflux solution and being centrifuged 11 minutes with 6000rpm, is washed with deionized 5 times.
4) take 2.2ml step 3) acquired solution that 6.2ml n,N-Dimethylformamide mixing ultrasonic treatment 15min is added.
5) gold electrode 1,2,3 with 0.02 μm of Al2O3After polishing, it is cleaned by ultrasonic with deionized water, is handled with 32 μ L step 4)
After solution afterwards is added drop-wise to gold electrode surfaces, dry in air.
6) by step 5) treated electrode 1,2,3, which are placed in 12 μ L, is diluted in 1000 times of Bombyx mori silk fibroin antibody,
It is rinsed after being incubated for 7h in 4 DEG C of environment with 7.4 buffer of PBS, then 32min is incubated for 1wt%BSA solution, with PBS 7.4
Buffer rinses.
The wherein preparation of 7.4 buffer of PBS: weighing 0.2 g potassium chloride, 0.27 g potassium dihydrogen phosphate, 8 g sodium chloride and
1.42 g disodium hydrogen phosphates are added to uniform stirring in 800 mL deionized waters until after being completely dissolved extremely with volumetric flask constant volume
1000 mL adjust the pH to 7.4 of solution.
9) take 9.6 buffer of Bombyx mori silk fibroin powder CB that extracts in step 2 at the fibroin of 100 μ g/mL
Protein solution；It takes 0.2g historical relic sample to be dissolved in 9.6 buffer of 100ml CB, is mixed evenly, stand, take supernatant.
The wherein preparation of 9.6 solution of CB: weighing 1.5 g sodium carbonate and 2.9 g sodium bicarbonates be added to 800 mL go from
Uniform stirring in sub- water adjusts the pH to 9.6 of solution until with volumetric flask constant volume to 1000 mL after being completely dissolved.
8) it takes in step 7) on 12 μ L of the silk fibroin protein solution electrode 1 that is added dropwise in step 6) that treated, takes in step 7)
On 12 μ L of historical relic sample solution is added dropwise in step 6) that treated electrode 2, and it is incubated for 70min under 37 DEG C of moist environment, used
7.4 buffer of PBS rinses.
9) electrode 3 of step 6) of learning from else's experience processing and the electrode 1,2 of step 8) processing, in 5Mm [Fe (CN)6]3-/4-In solution
Electrochemical Detection is carried out, scanning current potential is -0.2-0.6V, and amplitude 0.05V, gold electrode is as working electrode, platinum electrode conduct
Auxiliary electrode, saturated calomel electrode is as reference electrode；The difference that 1,3 gained current peak of electrode is occurred is as control, such as
There is difference in 2,3 current peak of fruit electrode, illustrates that historical relic sample contains mulberry silk, on the contrary then explanation does not have.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field；In the present invention
Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention
Technical spirit any simple modification, change and equivalent transformation to the above embodiments, still fall within the technology of the present invention side
The protection scope of case.
Claims (6)
1. a kind of method for detecting Ancient Silk Textile, which is characterized in that in terms of g, mg and mL, comprising the following steps:
1) it weighs 4-6g mulberry silk to be placed in sodium carbonate liquor of the 180-220mL containing 0.018-0.022M, water-bath 55-65min, water
Bath temperature is 75-85 DEG C, and taking-up is cleaned more than three times with deionized water, dry；
2) formic acid 48-52mL is added in the fibroin for taking 1.8-2.2g to dry, 2.3-2.7g calcium nitrate, stirs 80-100min, filtering
Addition sodium bicarbonate is in neutrality up to solution, after dialysis freeze-drying, obtained fibroin albumen is pulverized spare, is obtained silk
Fibroin powder；
3) taking 2.8-3.2mL concentration is that the graphene oxide of 5-7mg/mL is immersed in 0.2-0.4M propane diamine the 2.8- that flows back
3.2h；Then the sodium chloroplatinate of 5-6ml 0.1%(w/v) is added, continuously stirs and in identical temperature reflux 20-40min
Afterwards by 5-7mL 1%w/v sodium borohydride be added dropwise in reaction system, and at the same temperature further reflux 20-
40min is washed with deionized 3-5 times after cooling down final reflux solution and being centrifuged 9-11min with 5000-6000rpm；
4) 1.8-2.2ml step 3) acquired solution is taken to mix ultrasonic treatment 10- with 5.8-6.2ml n,N-Dimethylformamide
20min；
5) electrode 1,2,3 respectively with 0.02 μm of Al2O3After polishing, it is cleaned by ultrasonic with deionized water, with 28-32 μ L step 4) institute
After solution is added drop-wise to electrode surface, dry in air；
6) by step 5) treated electrode 1,2,3, which are placed in 8-12 μ L, is diluted in 1000 times of Bombyx mori silk fibroin antibody,
It is rinsed after being incubated for 5-7h in 1-5 DEG C of environment with 7.4 buffer of PBS, is then incubated for 28-32min with the BSA solution of 1wt%, uses
7.4 buffer of PBS rinses；
7) fibroin protein powder obtained by step 2 is taken, with 9.6 buffer of CB at the silk fibroin protein solution of 90-110 μ g/mL；
It takes 0.02-0.2g historical relic sample to be dissolved in 9.6 buffer of 100ml CB, is mixed evenly, stand, take supernatant；
8) it takes in step 7) on the silk fibroin protein solution 8-12 μ L electrode 1 that is added dropwise in step 6) that treated, takes step 7) Chinese
On object sample solution 8-12 μ L is added dropwise in step 6) that treated electrode 2, and 50- is incubated under 37 DEG C of moist environment
70min is rinsed with 7.4 buffer of PBS；
9) gold electrode 3 of step 6) of learning from else's experience processing and the electrode 1,2 of step 8) processing, in 5Mm [Fe (CN)6]3-/4-In solution into
Row Electrochemical Detection, scanning current potential are -0.2-0.6V, amplitude 0.05V；The difference that 1,3 gained current peak of electrode is occurred
As control, if difference occurs in 2,3 current peak of electrode, illustrate that historical relic sample contains mulberry silk, on the contrary then explanation is without containing silkworm
Silk.
2. a kind of method for detecting Ancient Silk Textile according to claim 1, it is characterized in that: filtering gained is molten in step 2
The cellulose dialysis bag that liquid is 8000-10000 with molecular cut off is dialysed 2-3 days in deionized water, and changes one every 5-7h
Secondary water, by silk fibroin protein solution vacuum refrigeration 2-3 days.
3. a kind of method for detecting Ancient Silk Textile according to claim 1, it is characterized in that: in step 3), reflux temperature is
65-75℃。
4. a kind of method for detecting Ancient Silk Textile according to claim 1, it is characterized in that: in step 6) and step 8), PBS
The preparation method of 7.4 buffers are as follows: weigh 0.2 g potassium chloride, 0.27 g potassium dihydrogen phosphate, 8 g sodium chloride and 1.42 g phosphoric acid
Disodium hydrogen is added to uniform stirring in 800 mL deionized waters until with volumetric flask constant volume to 1000 mL after being completely dissolved, and adjusts
The pH to 7.4 of solution.
5. a kind of method for detecting Ancient Silk Textile according to claim 1, it is characterized in that: 9.6 solution of CB in step 7)
Preparation method are as follows: weigh 1.5 g sodium carbonate and 2.9 g sodium bicarbonates be added to uniform stirring in 800 mL deionized waters until
With volumetric flask constant volume to 1000 mL after being completely dissolved, the pH to 9.6 of solution is adjusted.
6. a kind of method for detecting Ancient Silk Textile according to claim 1, it is characterized in that: in step 9), Electrochemical Detection
Comprising three electrodes, gold electrode is as working electrode, and platinum electrode is as auxiliary electrode, and saturated calomel electrode is as reference electrode.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104459162A (en) * | 2014-12-31 | 2015-03-25 | 浙江理工大学 | Method for preparing indirect competition method test paper for antique silk fabric |
| CN104483476A (en) * | 2014-12-31 | 2015-04-01 | 中国丝绸博物馆 | Detection method for ancient muddy silk fabric simulation sample |
| CN104483479A (en) * | 2014-12-31 | 2015-04-01 | 浙江理工大学 | Dot immunogold filtration assay method for testing antique silk fabric |
| CN107389641A (en) * | 2017-08-01 | 2017-11-24 | 浙江理工大学 | A kind of method based on immune vestige method detection ancient times argillization silk goods |
| CN108387435A (en) * | 2018-01-30 | 2018-08-10 | 中国计量大学 | A kind of trace fibroin albumen enrichment method |
-
2018
- 2018-09-05 CN CN201811028705.9A patent/CN109187699B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104459162A (en) * | 2014-12-31 | 2015-03-25 | 浙江理工大学 | Method for preparing indirect competition method test paper for antique silk fabric |
| CN104483476A (en) * | 2014-12-31 | 2015-04-01 | 中国丝绸博物馆 | Detection method for ancient muddy silk fabric simulation sample |
| CN104483479A (en) * | 2014-12-31 | 2015-04-01 | 浙江理工大学 | Dot immunogold filtration assay method for testing antique silk fabric |
| CN107389641A (en) * | 2017-08-01 | 2017-11-24 | 浙江理工大学 | A kind of method based on immune vestige method detection ancient times argillization silk goods |
| CN108387435A (en) * | 2018-01-30 | 2018-08-10 | 中国计量大学 | A kind of trace fibroin albumen enrichment method |
Non-Patent Citations (1)
| Title |
|---|
| BING WANG等: "Development of an Enzyme-Linked Immunosorbent Assay and Gold-Labelled Immunochromatographic Strip Assay for the Detection of Ancient Wool", 《JOURNAL OF ANALYTICAL METHODS IN CHEMISTRY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113740540A (en) * | 2021-09-03 | 2021-12-03 | 浙江理工大学 | Preparation method of organic electrochemical transistor for silk fibroin detection |
| CN113740540B (en) * | 2021-09-03 | 2024-05-03 | 浙江理工大学 | Preparation method of organic electrochemical transistor for silk fibroin detection |
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