Fingerprint spectrum detection method for ivory scraps in tin powder

A technology of fingerprint spectrum and detection method, which is applied in the field of fingerprint spectrum of traditional Chinese medicinal materials, can solve the problems such as the establishment and detection method of fingerprint spectrum that have not yet been found, and achieve the effects of controlling product quality, high precision and good separation effect.

Active Publication Date: 2021-04-27
JIANGSU 707 NATURAL PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there is no report on the establishment of fingerprints and detection methods for ivory shavings in tin powder

Method used

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  • Fingerprint spectrum detection method for ivory scraps in tin powder
  • Fingerprint spectrum detection method for ivory scraps in tin powder
  • Fingerprint spectrum detection method for ivory scraps in tin powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Three kinds of amino acid content change analysis in embodiment 1 ivory shavings

[0058] 1. Preparation of reference solution

[0059]Take appropriate amount of glycine, alanine, and leucine reference substances, weigh them accurately, add 0.1mol / L hydrochloric acid solution to prepare mixed reference substance stock solutions containing 800 μg of glycine, 400 μg of alanine, and 200 μg of leucine per 1 mL. Precisely measure 100 μL of the mixed reference substance stock solution and place it in a 2 mL vial, add 50 μL each of 14% triethylamine acetonitrile solution and phenylisothiocyanate acetonitrile solution (25 μL / 2 mL) successively, cover, mix well, and place in ( Derivatize at 28±0.5)°C for 90 minutes, take it out, add 400 μL of n-hexane, shake it, let it stand for 10 minutes, take the lower layer solution, and obtain it.

[0060] 2. Preparation of the test solution

[0061] Weigh about 150mg of ivory chip powder, weigh it accurately, add 5mL of 6mol / L hydrochlor...

Embodiment 2

[0067] The investigation of embodiment 2 experimental conditions

[0068] 1. Inspection of chromatographic system

[0069] (1) Inspection of detection wavelength

[0070] Investigate and detect the influence that detection wavelength is respectively 230nm, 254nm, 280nm the influence of each chromatographic peak separation situation in the tooth dust HPLC fingerprint chromatogram, except detection wavelength, all the other chromatographic conditions are all according to the condition sample introduction analysis of embodiment 1, record each chromatogram, Such as figure 2 shown.

[0071] The results show that when the detection wavelength is 280nm, the baseline of the spectrum shows a downward trend after 30min; The larger the number, the better the separation, so 254nm was finally selected as the detection wavelength.

[0072] (2) Investigation of mobile phase system

[0073] Investigate mobile phase system respectively when acetonitrile-0.01mol / L sodium acetate aqueous s...

Embodiment 3

[0120] The fingerprint spectrum detection method of embodiment 3 ivory chips

[0121] 1. Investigation of Fingerprint Methodology

[0122] (1) Precision

[0123] Get the ivory chip sample to be tested, prepare reference substance solution and need testing solution by the method of embodiment 1 respectively, accurately draw need testing solution 2 μ L, continuous sample injection 6 times, measure HPLC chromatogram, visually observe the full picture of fingerprint spectrum Obvious changes, using the "Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System" (version 2004A) issued by the National Pharmacopoeia Commission to calculate the similarity between the 6 chromatographic fingerprints and the obtained common pattern spectra, the full spectrum similarity is 1.000, indicating the precision of the instrument good.

[0124] (2) Repeatability

[0125] Get the ivory chip sample to be tested, prepare 6 parts of need testing solution in parallel according to the...

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Abstract

The invention discloses a fingerprint spectrum detection method for ivory scraps in tin powder. The method comprises the following steps of: (1) preparing a reference substance solution; (2) preparing a test solution; (3) defining chromatographic conditions; (4) establishing a standard fingerprint taking alanine as a reference peak; and (5) performing similarity evaluation. According to the method, the pretreatment method of each test sample is simple, the characteristic components are completely reserved, the repeatability and the stability are good, the precision is high, and the separation effect of each characteristic peak in an obtained fingerprint spectrum is good; and the product quality can be effectively controlled through the method.

Description

technical field [0001] The invention belongs to the technical field of fingerprints of traditional Chinese medicinal materials, and in particular relates to a fingerprint detection method of ivory chips in tin powder. Background technique [0002] Fingerprint of traditional Chinese medicine refers to the chromatogram or spectrum that can mark the chemical characteristics of some traditional Chinese medicinal materials or preparations after proper treatment and certain analysis methods. Traditional Chinese medicine fingerprint is a comprehensive and quantifiable means of identification. It is based on the systematic research on the chemical components of traditional Chinese medicine and is mainly used to evaluate the authenticity, goodness and stability of the quality of Chinese medicinal materials and semi-finished products of traditional Chinese medicine preparations. "Integrity" and "ambiguity" are its salient features. [0003] Xileisan is included in the drug standard o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/34G01N30/86
CPCG01N30/02G01N30/06G01N30/14G01N30/34G01N30/8675
Inventor 贺敬竹
Owner JIANGSU 707 NATURAL PHARMA
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