A method for establishing the uplc fingerprint of compound sarsaparilla granules

A technology of fingerprints and establishment methods, which is applied in the field of establishment of UPLC fingerprints of compound smilax granules, which can solve problems such as difficulty in establishing quality control standards for compound smilax granules and unlinking, so as to achieve comprehensive monitoring of product quality and shorten analysis time , good separation effect

Active Publication Date: 2021-07-23
GUOHUA PHARMACY HUNAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the basis of pharmacodynamic studies, there are few reports on the chemical composition analysis and fingerprints of the whole prescription, and it is difficult to establish a comprehensive and effective quality control standard for compound sarsaparilla granules, and the fingerprints are mainly related to quality control at present. , did not correlate certain characteristic components of the chromatographic fingerprint peaks with therapeutic efficacy

Method used

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  • A method for establishing the uplc fingerprint of compound sarsaparilla granules
  • A method for establishing the uplc fingerprint of compound sarsaparilla granules
  • A method for establishing the uplc fingerprint of compound sarsaparilla granules

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Embodiment 1 The establishment of fingerprint spectrum

[0047] 1. Configuration of sample solution

[0048] ) Sample solution configuration: Precisely weigh 1.0g each of 10 batches of compound Smilax granules S1~S10, add methanol to make up to 10mL, airtight, ultrasonically dissolve (250W, 40kHz), let cool, make up for weight loss with methanol, shake well , filtered, and the filtrate was filtered with a 0.22 μm filter membrane to obtain a total of 10 batches of sample solutions of compound Smilax granules from S1 to S10.

[0049] ) The configuration of the mixed reference solution: take chlorogenic acid, neochlorogenic acid, cryptochlorogenic acid, isoquercitrin, hyperoside, astilbin, 3,4-dicaffeoylquinic acid, 3,5 - Dicaffeoylquinic acid, appropriate amount of 4,5-dicaffeoylquinic acid reference substance, made by adding appropriate amount of methanol, containing 90 μg / mL of chlorogenic acid, 102.7 μg / mL of neochlorogenic acid, and 72.8 μg of cryptochlorogenic acid ...

Embodiment 2

[0078] Common peak assignment in the fingerprint spectrum of embodiment 2

[0079] Prepare negative control solution: Weigh 15g of Smilax chinensis, 15g of Houttuynia cordata, 15g of cat’s claw, 15g of medlar, 15g of jujube (pitted), 5g of coltsfoot flower, and 5g of ground beetle, and decoct them respectively. In the process, add 940ml of water for the first time (decoction for 1.5h), add 752mL of water for the second time (decoction for 1h), combine the decoction, concentrate, and dry with a freeze dryer to obtain the extract, and then prepare the extract to contain The crude drug amount is the solution of 2.03mg / ml, obtains 6 kinds of negative control solutions

[0080]The 6 kinds of negative control solutions in step 1) were subjected to UPLC chromatographic analysis respectively according to the above-mentioned chromatographic conditions, and the spectra of the 6 kinds of negative control solutions were obtained, such as figure 2 As shown, the standard fingerprint is co...

Embodiment 3

[0081] Example 3 common peak identification

[0082] The test solution and the mixed reference solution, under the following test conditions, conduct UPLC-ESI-MS negative ion mode for chemical component analysis, and then identify the active component corresponding to the fingerprint peak;

[0083] The test conditions are: electrospray ion source (ESI); negative ion mode scanning; capillary voltage 4000 V; ion source temperature 350 ℃; atomizer pressure 276 kPa; dryer volume flow rate 6 L / min; cone hole 65 V; dryer The temperature was 350°C; the fragment voltage was 110 V; the mass scanning range was m / z 100-1000; the sampling frequency was 0.1 s, and the interval was 0.02 s; the collision energy was 15 eV. Before measuring the sample, use the tuning solution to calibrate the mass axis to ensure that the mass accuracy error is less than 1×10-6.

[0084] The detected retention time (tR), mass spectrometry information and cracking law were compared with the reference substance ...

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Abstract

The invention discloses a method for establishing the UPLC fingerprint of compound sarsaparilla granules and its fingerprint and application, which comprises the following steps: (1) sample preparation: ① preparation of a test solution; ② preparation of a mixed reference solution; 2) UPLC fingerprint of compound Smilax granule extract: Take 2 μL each of the test solution and the mixed control solution, respectively inject UPLC chromatographic analysis, measure under the set chromatographic conditions, record the chromatogram for 38 minutes, and obtain the fingerprint. The invention establishes the UPLC fingerprint of the compound smilax granule. Compared with HPLC, the UPLC can greatly shorten the analysis time of the fingerprint while ensuring good separation of the compound smilax granule extract. The fingerprint components of the compound sarsaparilla granules of the present invention are kept intact, and have 18 common peaks, which have been identified and analyzed. The separation effect of each characteristic peak is good, and the quality information of the product can be reflected more comprehensively. It is beneficial to comprehensively monitor product quality and identify the authenticity of products.

Description

technical field [0001] The invention belongs to the technical field of fingerprint analysis of traditional Chinese medicines, and in particular relates to a method for establishing UPLC fingerprints of compound sarsaparilla granules. Background technique [0002] Fingerprint refers to certain complex substances, such as traditional Chinese medicine, the DNA of a certain organism or a certain tissue or cell, and after the protein is properly processed, the chromatogram or spectrum that can mark its chemical characteristics is obtained by using certain analysis methods. . Traditional Chinese medicine fingerprint is a comprehensive and quantifiable means of identification. It is based on the systematic study of the chemical components of traditional Chinese medicine and is mainly used to evaluate the authenticity, excellence and stability of the quality of Chinese medicinal materials and Chinese medicinal preparations. Traditional Chinese medicine and its preparations are mult...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 朱立华陈林张水寒胥新元
Owner GUOHUA PHARMACY HUNAN
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