A method for detecting ancient silk fabrics

A technology of silk fabrics and silk fibroin, which is applied in the field of cultural relics detection, can solve the problems of high impurity interference, unsuitability for cultural relics detection, low sensitivity, etc., and achieve the effects of enhanced sensitivity, excellent sensitization and modifiability, and high sensitivity

Active Publication Date: 2020-06-23
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And as an organic polymer material, mulberry silk is easily degraded by light, heat, acid-base, microorganisms, etc., resulting in changes in crystallinity, molecular weight and other structure and properties. Therefore, conventional detection methods have low sensitivity and are interfered by impurities. It has a large impact and is not suitable for detecting cultural relics. Therefore, it is necessary to develop a method for detecting ancient silk fabrics with good sensitivity and specificity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Weigh 5g of mulberry silk and place it in 180mL of 0.018M sodium carbonate solution, bathe in water for 55min at a temperature of 80°C, take it out and wash it with deionized water three times, and put it in an oven to dry.

[0029] 2) Take 2g of dried silk fibroin and 2.3g of calcium nitrate, add 48mL of formic acid, stir with magnetic force for 80min, filter and add sodium bicarbonate until the solution is neutral, and use a cellulose dialysis bag with a molecular weight cut-off of 8000 to remove the obtained solution. Dialyze in deionized water for 2 days, and change the water every 5 hours, freeze-dry the silk fibroin solution in a vacuum freeze dryer for 2 days, and grind the obtained silk fibroin into powder for later use.

[0030] 3) Take 2.8mL of graphene oxide with a concentration of 5mg / mL soaked in 0.2M propylenediamine and reflux at 65°C for 2.8h; then, add 5ml of 0.1% (w / v) sodium hexachloroplatinate to the previously After stirring continuously and refl...

Embodiment 2

[0040] 1) Weigh 5g of mulberry silk and place it in 200mL of 0.02M sodium carbonate solution, bathe in water for 60min at a temperature of 80°C, take it out and wash it four times with deionized water, and put it in an oven to dry.

[0041] 2) Take 2g of dried silk fibroin and 2.5g of calcium nitrate, add 50mL of formic acid, stir with magnetic force for 90min, filter and add sodium bicarbonate until the solution is neutral, and use a cellulose dialysis bag with a molecular weight cut-off of 9000 to remove the obtained solution. Dialyze in deionized water for 2.5 days, and change the water every 6 hours, freeze-dry the silk fibroin solution in a vacuum freeze dryer for 2.5 days, and grind the obtained silk fibroin into powder for later use.

[0042] 3) Take 3 mL of graphene oxide with a concentration of 6 mg / mL soaked in 0.3M propylenediamine and reflux at 70 °C for 3 h; then, add 5.5 mL of 0.1% (w / v) sodium hexachloroplatinate to the previous 6 mL of 1% w / v sodium borohydride...

Embodiment 3

[0052] 1) Weigh 5g of mulberry silk and place it in 220mL of 0.022M sodium carbonate solution, bathe in water for 65min at a temperature of 80°C, take it out and wash it with deionized water five times, and put it in an oven to dry.

[0053] 2) Take 2g of dried silk fibroin and 2.7g of calcium nitrate, add 52mL of formic acid, stir with magnetic force for 100min, filter and add sodium bicarbonate until the solution is neutral, and use a cellulose dialysis bag with a molecular weight cut-off of 10,000 to remove the obtained solution. Dialyze in deionized water for 3 days, and change the water every 7 hours, freeze-dry the silk fibroin solution in a vacuum freeze dryer for 3 days, and grind the obtained silk fibroin into powder for later use.

[0054] 3) Take 3.2mL of graphene oxide with a concentration of 7mg / mL soaked in 0.4M propylenediamine and reflux at 75°C for 3.2h; then, add 6ml of 0.1% (w / v) sodium hexachloroplatinate to the previously , continuously stirred and refluxe...

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PUM

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Abstract

The invention relates to the field of cultural relic detection and discloses a method for detecting an ancient silk fabric. The method comprises the following steps: extracting silk fibroin by adopting formic acid and a calcium nitrate solution system; then preparing a graphene nano compound modified working electrode through a mixed system of graphene oxide, propylene diamine, sodium hexachloroplatinate hexahydrate and sodium borohydride; successively modifying a silkworm silk fibroin antibody and a detected sample on the working electrode; and electrochemically detecting current value respectively, and judging whether the sample is the silk fabric or not through analyzing the changes of the current value. The method provided by the invention is simple to operate and high in sensitivity.

Description

technical field [0001] The invention relates to the field of cultural relic detection, in particular to a method for detecting ancient silk fabrics. Background technique [0002] China has been a big country of textiles since ancient times. The textiles produced are rich in variety, exquisite in craftsmanship, comfortable and breathable. Among them, the most famous textile is Chinese silk, so China is also known as the "Country of Silk". The main component of silk is mulberry silk, which is mainly composed of silk fibroin and sericin. Silk fibroin is the main component of silk, accounting for about 70% of the total weight. And as an organic polymer material, mulberry silk is easily degraded by light, heat, acid-base, microorganisms, etc., resulting in changes in crystallinity, molecular weight and other structure and properties. Therefore, conventional detection methods have low sensitivity and are interfered by impurities. It has a large impact and is not suitable for det...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/416
CPCG01N27/416
Inventor 王秉李青青刘林帅欧阳毅彭志勤胡智文
Owner ZHEJIANG SCI-TECH UNIV
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