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Method for establishing fingerprint of Ferula sinkiangensis K. M. Shen polysaccharide by utilizing HPLC-MS

A fingerprint and polysaccharide technology, applied in the field of traditional Chinese medicine fingerprints, can solve the problems of increasing the difficulty of establishing traditional Chinese medicine fingerprints, few qualitative researches on characteristic common peaks, and the reliability of fingerprints needs to be improved, so as to promote quality improvement and stability. , improve the accuracy and sensitivity, reliability and high precision effect

Inactive Publication Date: 2019-03-05
MINZU UNIVERSITY OF CHINA
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Problems solved by technology

However, the diversity and complexity of the chemical components of traditional Chinese medicine and the uncertainty of the substance basis of the medicinal effect increase the difficulty of establishing the fingerprint of traditional Chinese medicine, as well as the validity and reproducibility of the fingerprint
[0005] At present, most studies on the fingerprints of ferulicum in Xinjiang focus on the establishment of HPLC fingerprints of volatile oils, water extracts and ethanol extracts. However, due to the limitations of chromatographic qualitative analysis, there are few qualitative studies on the characteristic common peaks, and the fingerprints are credible. Degree to be improved
In addition, quality control and quality evaluation of Chinese herbal medicines using fingerprints established by only a single method will inevitably lead to missing information and biased evaluation results, making it difficult to form a clear and complete understanding of such a complex system as traditional Chinese medicine

Method used

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  • Method for establishing fingerprint of Ferula sinkiangensis K. M. Shen polysaccharide by utilizing HPLC-MS
  • Method for establishing fingerprint of Ferula sinkiangensis K. M. Shen polysaccharide by utilizing HPLC-MS
  • Method for establishing fingerprint of Ferula sinkiangensis K. M. Shen polysaccharide by utilizing HPLC-MS

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Experimental program
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Effect test

Embodiment 1

[0069] Embodiment 1, establishment of monosaccharide standard curve

[0070] 1. Preparation of monosaccharide standard solution

[0071] Accurately weigh 1 mg of each of the 10 monosaccharide standard substances, place them in stoppered test tubes, and add 1 mL of ultrapure water to dissolve completely.

[0072] The 10 kinds of monosaccharide standard solutions were derivatized with PMP respectively: add 1mL 0.3mol / L NaOH solution and 1mL 0.5mol / L PMP methanol solution to the corresponding 1mL 1mg / mL monosaccharide standard solution respectively, stopper and seal in a 70℃ water bath React for 1h, take it out and let it cool to room temperature; add 1mL 0.3mol / L HCl solution to shake and neutralize, add ultrapure water to 5mL, and then add 5mL CHCl 3 , vibrate, stand still, discard the organic phase, and extract like this 3 times until the organic phase is transparent and colorless. Pass the aqueous phase through a 0.22 μm microporous membrane and wait for sample injection. ...

Embodiment 2

[0093] Embodiment 2, the establishment of Xinjiang ferulicum polysaccharide fingerprint

[0094] 1. Establishment and evaluation of Xinjiang ferulicum polysaccharide fingerprint

[0095] (1) Determination of common peaks

[0096] Collect 9 batches of Xinjiang Ferulica samples and operate according to the steps of polysaccharide extraction, complete hydrolysis, and PMP derivatization in Example 1, and analyze under the above-mentioned detection conditions to obtain the chromatograms of each batch of samples. The results are as follows figure 2 shown. Comparing the chromatograms obtained by each batch, it is determined that there are 5 common characteristic peaks, and the Xinjiang Ferula polysaccharide spectrum data of each batch is generated by the average number method, and the common pattern is used as the Xinjiang Ferula HPLC-MS fingerprint Atlas (see attached image 3 ), this fingerprint is compared with the retention time of standard monosaccharide sample and sample, qu...

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Abstract

The invention relates to a method for establishing a fingerprint of Ferula sinkiangensis K. M. Shen polysaccharide by utilizing HPLC-MS. The method for establishing the fingerprint of Ferula sinkiangensis polysaccharide by utilizing an HPLC-MS technology is used by combining the separation function of a chromatography and the qualitative determination function of a mass spectrum, thereby greatly improving accuracy and sensitivity of quality detection. Meanwhile, the method provided by the invention establishes the quantitative fingerprint of water-soluble Ferula sinkiangensis polysaccharide for the first time, can utilize the mass spectrum for accurate qualitative determination of a common peak, can accurately calculate the peak area of peaks through extraction of an ion chromatogram for qualitative determination, and is more effective to establish the fingerprint from two levels. The method provided by the invention has high sensitivity and strong specificity, and can be used as one of the important means for identification and quality evaluation of a Ferula sinkiangensis medicinal material.

Description

technical field [0001] The invention relates to a method for establishing Xinjiang Ferulicum polysaccharide fingerprints by using HPLC-MS and a standard fingerprint of Xinjiang Ferulic polysaccharides obtained by the method, belonging to the technical field of traditional Chinese medicine fingerprints. Background technique [0002] Ferula sinkiangensis (Ferula sinkiangensis K.M.Shen) is a perennial herb belonging to the family Umbelliferae (Umbelliferae). It has the effects of eliminating stagnation, dispelling lumps, killing insects, dispelling dampness, and relieving pain. It is used to treat stagnation of meat, blood stasis, abdominal pain and other diseases. Xinjiang Asafoetida is mainly produced in Xinjiang and has a long history of application. The 1977 edition of "Chinese Pharmacopoeia" stipulates that there are only two species of Ferula ferulae (Ferulasinkiangensis K.M.Shen) and Ferula fukanensis (Ferula fukanensis K.M.Shen) as traditional Chinese medicine. Tradit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/86G01N30/88G01N30/06
CPCG01N30/06G01N30/8686G01N30/88
Inventor 刘春兰黄雅婷岳丽君申翔宇王坤
Owner MINZU UNIVERSITY OF CHINA
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