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Fingerprint map and high performance liquid chromatography identification method for Xuezhitong capsule

A high-performance liquid chromatography and fingerprint technology, which is applied in the identification of Xuezhitong Capsules by high-performance liquid chromatography and the establishment of Xuezhitong Capsules' fingerprints, can solve the problems of instability and errors of sulfur-containing compounds, and achieve a moderate ratio. , uniform distribution, good overall fingerprint effect

Active Publication Date: 2017-09-26
吉林省东方制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the Xuezhitong Capsules standard includes one item of thin layer identification and one item of content determination; the content determination item is the measurement item of combined sulfur content. However, due to the instability of sulfur-containing compounds, this method has a large error

Method used

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  • Fingerprint map and high performance liquid chromatography identification method for Xuezhitong capsule
  • Fingerprint map and high performance liquid chromatography identification method for Xuezhitong capsule
  • Fingerprint map and high performance liquid chromatography identification method for Xuezhitong capsule

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Example 1 Establishment of Xuezhitong Capsule Fingerprint

[0060] 1. Experimental materials

[0061] 1.1 Sample

[0062] 血滞通胶囊由吉林省东方制药有限公司提供,共20批,批号分别为:20120804、20120810、20120903、20120906、20120907、20130102、20130103、20130104、20130105、20130706、20130707、20130902、20140408、20140409、20140410 , 20150101, 20150502, 20150503, 20150603, 20150604. There are 4 batches of allium medicinal materials, the batch numbers are: YZ-31-150501, YZ-31-141101, YZ-31-140901, YZ-31-140801. 4 batches of intermediates, the batch numbers are: 20150514, 20150601, 20150602, 20150603.

[0063] 1.2 Instruments and reagents

[0064] 1.2.1 Instruments

[0065] Shimadzu LC-20AT high performance liquid chromatography, LC-solution workstation (Shimadzu, Japan). Chinese medicine fingerprint similarity evaluation system software version 2.0; Agilent 1200Series high performance liquid chromatograph, Agilent Chem Station chromatographic workstation (Agilent, USA). KQ-200 Ultrasonic Cleaner (Kunshan Shum...

Embodiment 2

[0142] The high-performance liquid chromatography identification of embodiment 2 Xuezhitong Capsules

[0143] 1, experimental material is the same as embodiment 1 fingerprint spectrum research.

[0144] 2. The preparation of the test solution is the same as the fingerprint research in Example 1.

[0145] 3. The chromatographic experiment conditions are the same as those in Example 1 for fingerprint research.

[0146] 4. The screening of the preparation conditions of the test product is the same as in Experimental Example 1.

[0147] 5. Methodological validation

[0148] 5.1 Precision test: the same as in Example 1 for fingerprint research.

[0149] 5.2. Stability test: the same as in Example 1 for fingerprint research.

[0150] 5.3 Repeatability test: the same as in Example 1 for the fingerprint study.

[0151] 5.4 Specificity test

[0152] The prescription of Xuezhitong Capsules only contains the medicinal material Allium scallions, and the others are auxiliary material...

experiment example 1

[0158] Experimental Example 1 Screening of Preparation Conditions of Test Articles in the Establishment of Xuezhitong Capsules Fingerprint

[0159] 1. Selection of extraction solvent

[0160] The present invention has selected 30% methanol, 50% methanol, methyl alcohol, 50% ethanol and ethanol (both volume percent) to extract Xuezhitong capsules, contrast HPLC chromatographic peaks (other parameters and chromatographic experiment conditions for test solution preparation) All with embodiment 1). the result shows( Figure 28 ), 50% methanol as the extraction solvent has the largest chromatographic peak area, the best extraction efficiency, and the best overall appearance. Therefore, the present invention selects 50% methanol as the extraction solvent of Xuezhitong capsules.

[0161] 2. Selection of extraction method

[0162] The present invention respectively ultrasonically extracts once for 30 minutes, ultrasonically extracts twice for 30 minutes (power 250W, frequency 40KH...

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Abstract

The invention discloses a fingerprint map and high performance liquid chromatography identification method for a Xuezhitong capsule. The invention firstly discloses an establishing method of a Xuezhitong capsule fingerprint map. The establishing method comprises the following steps: (1) adding a Xuezhitong capsule content in an extraction solvent for extraction to obtain an extracting solution, and purifying the extracting solution to obtain a test sample solution; (2) performing high performance liquid chromatographic analysis on the test sample solution to acquire a high performance liquid chromatogram; and (3) selecting a common peak from chromatographic peaks in the high performance liquid chromatogram to obtain the Xuezhitong capsule fingerprint map. The invention further discloses the Xuezhitong capsule fingerprint map established by the method. The invention also discloses a Xuezhitong capsule high performance liquid chromatography identification method. The method can accurately identify adenosine and syringin in the Xuezhitong capsule and is good in accuracy, stability and repeatability. The fingerprint map and high performance liquid chromatography identification method for the Xuezhitong capsule, established by the invention, has an application prospect in quality control of the Xuezhitong capsule.

Description

technical field [0001] The present invention relates to a method for establishing the fingerprints of Xuezhitong capsules, and also relates to the fingerprints of Xuezhitong capsules established by the method. The present invention further relates to a high-performance liquid chromatography identification method for Xuezhitong capsules, which belongs to Xuezhitong capsules. The field of identification of Tong capsules. Background technique [0002] Xuezhitong Capsules are capsules processed from Allium scallops, the contents are light brown granules and powder, with garlic odor and slightly spicy taste; functions and indications: clearing yang and dispelling stagnation, promoting qi and guiding stagnation; used for hyperlipidemia Chest tightness, fatigue, abdominal distension, etc. caused by blood stasis and phlegm obstruction. [0003] At present, the Xuezhitong Capsule standard includes one item of thin layer identification and one item of content determination; the conte...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/8809
Inventor 李文革杨德辉
Owner 吉林省东方制药有限公司
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