Silk cultural relic fiber material identification method based on amino acid analysis

A technology for amino acids and cultural relics, applied in the direction of analyzing materials, material separation, measuring devices, etc., can solve problems such as limitations in identification, and achieve the effect of less sample demand

Inactive Publication Date: 2013-09-18
CHINA NAT SILK MUSEUM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Different varieties of silk have different molecular structures. Due to the change of molecular structure caused by the aging and degradation of silk cultural relics, the sensitivity of infrared spectroscopy analysis has limitations for the identification of silk of the same species.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A method for identifying silk cultural relic fiber material based on amino acid analysis, which adopts the following steps:

[0023] A) Weigh 0.3 mg silk cultural relic sample, put it into a hydrolysis test tube, dissolve it in 0.5ml 6N HCl, seal the test tube mouth while vacuuming, and hydrolyze the sample at 110°C for 22-24 hours.

[0024] B) The hydrolyzed sample was blown dry with a nitrogen blower, reconstituted with 1.5ml of 0.1N HCl, freeze-dried at -20°C and stored until chromatographic analysis.

[0025] C) Use the AQC amino acid analysis package and 2695HPLC of Waters Company of the United States to separate and detect amino acids.

[0026] D) Data processing, using the relative mole percentage to characterize the content of each amino acid. When the molar ratio of glycine:alanine:serine is 4:3:1, it can be inferred that the fiber material of the silk cultural relic is silk; when the molar ratio of glycine:alanine:serine is 3:4:1, It can be inferred that the...

Embodiment 2

[0028] A method for identifying silk cultural relic fiber material based on amino acid analysis, which adopts the following steps:

[0029] A) Weigh 0.4 mg silk cultural relic sample, put it into a hydrolysis test tube, dissolve it in 1.0ml 6N HCl, seal the test tube mouth while vacuuming, and hydrolyze the sample at 110°C for 22-24 hours.

[0030] B) The hydrolyzed sample was blown dry with a nitrogen blower, reconstituted with 2.0ml 0.1N HCl, freeze-dried and stored at -20°C until chromatographic analysis.

[0031] C) Use the AQC amino acid analysis package and 2695HPLC of Waters Company of the United States to separate and detect amino acids.

[0032] D) Data processing, using the relative mole percentage to characterize the content of each amino acid. When the molar ratio of glycine:alanine:serine is 4:3:1, it can be inferred that the fiber material of the silk cultural relic is silk; when the molar ratio of glycine:alanine:serine is 3:4:1, It can be inferred that the fi...

Embodiment 3

[0034] A silk cultural relic fiber material identification method based on amino acid analysis is characterized in that the following steps are adopted:

[0035] A) Weigh 0.5 mg silk cultural relic sample, put it into a hydrolysis test tube, dissolve it in 1.5ml 6N HCl, seal the test tube mouth while vacuuming, and hydrolyze the sample at 110°C for 22-24 hours.

[0036] B) The hydrolyzed sample was blown dry with a nitrogen blower, reconstituted with 2.5ml of 0.1N HCl, freeze-dried and stored at -20°C until chromatographic analysis.

[0037] C) Use the AQC amino acid analysis package and 2695HPLC of Waters Company of the United States to separate and detect amino acids.

[0038] D) Data processing, using the relative mole percentage to characterize the content of each amino acid. When the molar ratio of glycine:alanine:serine is 4:3:1, it can be inferred that the fiber material of the silk cultural relic is silk; when the molar ratio of glycine:alanine:serine is 3:4:1, It ca...

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PUM

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Abstract

The invention discloses a silk cultural relic fiber material identification method based on amino acid analysis. The method comprises the following steps: (A) weighing 0.3-0.5mg of silk cultural relic sample in microgramme grade, putting the silk cultural relic sample in a hydrolysis test tube, dissolving the silk cultural relic sample in 0.5-1.5ml of 6NHCl, vacuumizing while sealing a test tube opening, hydrolyzing the sample for 22-24 hours at 110 DEG C; (B) drying the hydrolyzed sample by using a nitrogen blowing instrument, redissolving in 1.5-2.5ml of 10.1N HCl, freezing, drying and preserving at minus 20 DEG C till the chromatographic analysis is implemented; (C) performing ammonic acid separation and detection by using an AQC amino acid analysis packet and 2695HPLC of Waters company of America; (D) processing data, representing the content of each amino acid by utilizing relative mol percentage, when the mol ratio of the glycine to alanine to serine is 4: 3: 1, deducing that the fiber material of the silk culture relic is mulberry silk, when the mol ratio of the glycine to alanine to serine is 3: 4: 1, deducing that the fiber material of the silk culture relic is tussah silk. The variety and the content of the amino acid can be flexibly detected, and the culture relic cannot be greatly damaged since the sample quantity demand is few. The method disclosed by the invention is suitable for the identification of the silk cultural relic fiber material.

Description

technical field [0001] The invention relates to a silk cultural relic fiber material identification method based on amino acid analysis, and belongs to the technical field of textile cultural relic fiber material identification. Background technique [0002] China is an ancient country of silk civilization. In the long course of civilization, relying on the advantages of vast territory, rich fiber types and numerous sources, primitive collection, domestication of wild silkworms, silk reeling and silk weaving have created a brilliant silk weaving culture in the world. Silk fabrics in ancient my country were mainly woven from mulberry silk, but there were also some wild silk. Although both wild silk and domestic silk are protein fibers, they are different in composition and performance. Identifying the fiber material of silk cultural relics can make the search for cultural relics protection methods more targeted in the later stage. [0003] The commonly used identification m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 郑海玲周旸赵丰
Owner CHINA NAT SILK MUSEUM
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