Method for establishing Sishen tablet fingerprint spectrum

A technique for fingerprinting and establishing methods, which is applied to the quality control of Sishen tablets, fingerprints, and the construction of high-performance liquid phase fingerprints of Sishen tablets, to achieve good reproducibility, reduce the possibility of quality compliance, and high precision Effect

Inactive Publication Date: 2014-12-10
沈阳双鼎制药有限公司
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Problems solved by technology

At present, there is no report on the fingerprinting method of Sishen Tablets

Method used

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  • Method for establishing Sishen tablet fingerprint spectrum
  • Method for establishing Sishen tablet fingerprint spectrum
  • Method for establishing Sishen tablet fingerprint spectrum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: The fingerprint detection method of Sishen tablet comprises the following steps:

[0040] 1. Instruments and reagents

[0041] 1.1 Instruments Shimazu high performance liquid chromatography, LC-20 UV detector, Labsolution chromatography workstation.

[0042] 1.2 Reagents Psoralen, isopsoralen, schisandra alcohol A reference substance; acetonitrile (chromatographically pure), twice redistilled water, phosphoric acid (analytical pure).

[0043] 2. High performance liquid chromatography

[0044] 2.1 Chromatographic conditions: the chromatographic column is filled with octadecylsilane bonded silica gel, and the Phenomenex chromatographic column: C 18 (250 × 4.6 mm, 5 μm); using gradient elution, the mobile phase is gradient eluent composed of acetonitrile and water; column temperature: 35°C; detection wavelength: 246nm; flow rate: 1.0ml / min; injection volume: 10μL . The number of theoretical plates should not be less than 5000 according to the psoralen te...

Embodiment 2

[0051] Example 2 Detect the fingerprints of 10 batches of Sishen Tablets

[0052] Get 10 batches of Sishen Tablets, detect according to the conditions of Example 1, and obtain the HPLC collection of samples of 10 batches, such as image 3 shown. Through the comparison of 10 batches of HPLC chromatograms, the similarity evaluation is carried out, and the characteristic common peaks are determined:

[0053] There are 15 common peaks in the fingerprint spectrum. Now the retention time of the spectrum, the average value of the peak area and the proportion of the total area are as follows:

[0054] For peak No. 1, the average retention time RT is 3.21min, the RSD is 0.11%, the peak area is 129767, and the RSD is 15.27%, accounting for 3.28% of the total peak area.

[0055] For peak No. 2, the average retention time RT is 11.090min, the RSD is 4.09%, the peak area is 229612, and the RSD is 10.68%, accounting for 5.80% of the total peak area.

[0056] For peak No. 3, the average...

Embodiment 3

[0080] Example 3 Sishen Tablet Standard Fingerprint Spectrum and Common Peak Assignment

[0081] 3.1 Generation of standard fingerprints

[0082] Get 10 batches of Sishen Tablets, detect according to the conditions of Example 1, and obtain the HPLC collection of samples of 10 batches, such as Figure 5 shown. Adopt Chinese medicine chromatographic fingerprint atlas similarity evaluation system software (2004A edition) to carry out similarity evaluation, method is the same as embodiment 2, and generates standard fingerprint atlas, see Figure 5 .

[0083] 3.2 Assignment of common peaks in fingerprints

[0084] The fingerprints of each medicinal material in Sishen Tablets were determined according to the law, and they were imported into the fingerprint similarity evaluation software (Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System, 2004A version) with the comparison spectra of Sishen Tablets respectively. Indicate its contribution to the common pe...

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Abstract

The invention discloses a method for establishing a Sishen tablet preparation fingerprint spectrum. The method comprises the following steps: preparing a reference solution which contains 10-100mg of psoralen, isopsoralen and schisandrin per milliliter; and removing coatings from Sishen tablets, weighing out 0.1-10g of Sishen tablets without coating, performing ultrasonic extraction with methanol, performing filtration to obtain a test solution, precisely sucking the test solution, injecting the test solution into a liquid chromatograph, and determining in accordance with a liquid chromatography, thereby obtaining the fingerprint spectrum. The method is performed under the following chromatographic conditions: octadecyl silane-bonded silica gel serves as stuff of a chromatographic column, a mobile phase refers to a gradient eluent consisting of acetonitrile and water, the detection wavelength is 220-360nm, the column temperature is 20-50 DEG C, the flow velocity is 0.5-1.5ml/min and the time is 30-90 min. The method is simple and stable, has high precision and good reproducibility, and is capable of rapidly and correctly distinguishing the authenticity and the quality of products.

Description

technical field [0001] The invention relates to a quality control method for Sishen Tablets, in particular to a method for constructing high-efficiency liquid phase fingerprints and fingerprints of Sishen Tablets, and belongs to the technical field of traditional Chinese medicine. Background technique [0002] Fingerprint of traditional Chinese medicine refers to the use of modern analysis technology to characterize and describe the chemical information of traditional Chinese medicine in a graphical way. map. At present, the fingerprint quality control technology of traditional Chinese medicine, as a detection method to control the quality stability and uniformity of traditional Chinese medicine, is one of the key technologies in the modernization of traditional Chinese medicine, which is of great significance to effectively control the quality of traditional Chinese medicine. Chromatographic fingerprint quality control technology is the highlight of the current quality res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 马占芝生可心王学东姜峰王淞林
Owner 沈阳双鼎制药有限公司
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