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Construction method and application of Shenzhiling oral liquid fingerprint

A technology of Shenzhiling oral liquid and fingerprints, which is applied in the construction and application field of fingerprints of Shenzhiling oral liquid, can solve the problems of limited resolution and peak capacity, and achieve improved separation selectivity, good reproducibility, good separation effect

Active Publication Date: 2018-01-26
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for Shenzhiling oral liquid with many components, the resolution and peak capacity of the above method are relatively limited.

Method used

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  • Construction method and application of Shenzhiling oral liquid fingerprint
  • Construction method and application of Shenzhiling oral liquid fingerprint
  • Construction method and application of Shenzhiling oral liquid fingerprint

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0038] (1) Preparation of the test solution: take Shenzhiling Oral Liquid, add methanol, ultrasonically extract, refrigerate and place for 0.5-1 hour, return to room temperature, filter, and take the filtrate to obtain the test solution;

[0039] (2) Preparation of reference substance solution: take paeonifloride glucoside, paeoniflorin, liquiritin, cinnamic acid, and ammonium glycyrrhizinate reference substances dried under reduced pressure to constant weight, and add methanol respectively to prepare reference substance solutions;

[0040] (3) Determination: Accurately draw need testing solution and reference substance solution respectively, inject high performance liquid chromatograph and detect through HPLC separation, the composition of mobile phase is acetonitrile-0.1% phosphoric acid aqueous solution, adopts gradient elution, and chromatographic column is by C1( TMS) in series with C18 to form, and use fingerprint software to analyze and process the spectrum obtained by h...

Embodiment 1

[0059] Example 1: Construction and application of the fingerprint of Shenzhiling Oral Liquid based on double-column series connection

[0060] The chromatographic conditions are: the chromatographic column is YMC-Pack TMS (5μm, 100×4.6mm) in series with JADE-PAK ODS-AQ chromatographic column (5μm, 150×4.6mm); mobile phase: mobile phase A is 0.1% phosphoric acid aqueous solution, mobile Phase B is acetonitrile, elution method: gradient elution; flow rate 0.8ml / min, column temperature 30°C, detection wavelength 254nm, injection volume 10μl, theoretical plate number not less than 8000 based on the chromatographic peak of cinnamic acid, all groups The scores were tested within 90 minutes. Wherein, the mobile phase linear gradient is shown in Table 1:

[0061] Table 1 Gradient elution conditions of chromatographic mobile phase

[0062]

[0063] (1) Preparation of the test solution: Precisely measure 1.25ml of Shenzhiling Oral Liquid in a 25ml volumetric flask, add methanol to ...

Embodiment example 2

[0072] Implementation Case 2: Methodological Investigation

[0073] The methodological investigation mainly examined the precision, stability and repeatability. The inspection methods and results are as follows:

[0074] (1) Precision test The same batch of Shenzhiling Oral Liquid samples were taken. After pretreatment, under the optimal chromatographic conditions, the two-column direct series method was used to continuously measure 6 times and record the chromatograms. The results are shown in Table 3. It can be seen from the table that the relative retention time ratio of each main chromatographic peak has no obvious change, and the RSD is 0.037%-0.31%. Except for No. 14 chromatographic peak, the relative peak area RSD of each main chromatographic peak is 0.7%-4.2%, RSD<5.0%, indicating that the precision of the instrument is good. Because the common peak area of ​​No. 14 is small (<1% of the total area), its RSD value is relatively large.

[0075] (2) Stability test The s...

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Abstract

The invention discloses a construction method and an application of a Shenzhiling oral liquid fingerprint. The method comprises the following steps: production of a sample solution, production of a reference substance solution, optimization and determination of chromatographic conditions, determination of the fingerprint, and analysis of the obtained fingerprint of a Shenzhiling oral liquid. Chromatographic columns having different stationary phases are directly connected in series, the same mobile phase is used to carry out gradient elution, and multiple characteristic index components are well separated. Compared with existing fingerprint establishing methods, the above method can realize the separation and detection of possible many characteristic components of the Shenzhiling oral liquid to obtain many fingerprint characteristic peaks, allows the component information of the Shenzhiling oral liquid to be comprehensively reflected, has the advantages of simplicity in operation, highprecision, good stability and good repeatability, can provide a more effective and comprehensive method basis for controlling and evaluating the quality of the Shenzhiling oral liquid, and ensures the effectiveness and the safety of drugs.

Description

technical field [0001] The present invention relates to the field of high performance liquid chromatography utilization and the field of analysis quality control of traditional Chinese medicine preparations, in particular to a construction method and application of the fingerprint of Shenzhiling oral liquid, especially to an improved reference method established based on chromatographic columns in series. The construction method of HPLC fingerprint of Zhiling Oral Liquid and the application of the fingerprint obtained by this method in the quality control of Shenzhiling Oral Liquid. Background technique [0002] Shenzhiling Oral Liquid is made of ten medicinal materials such as Codonopsis pilosula, Guizhi, white peony root, licorice, Poria cocos, Shichangpu, polygala, dried ginger, keel, and oyster. Deficiency of heart-qi manifested in mild to moderate Alzheimer's disease mainly manifests as forgetfulness, palpitations, dizziness, insomnia, lack of breath, trouble speaking, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 聂磊姜文文臧恒昌曾英姿姜红
Owner SHANDONG UNIV
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