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Fingerprint spectrum of immature bitter orange medicinal material and construction method and application of fingerprint spectrum

A technique for fingerprinting and establishing methods, which is applied in the field of pharmaceutical analysis, can solve problems such as the inability to fully reflect the types and quantities of internal chemical components of traditional Chinese medicine, and the complexity of methods for determining the content of synephrine, and achieve good stability and reproducibility

Active Publication Date: 2014-06-04
INST OF PHARMACOLOGY & TOXICOLOGY ACAD OF MILITARY MEDICAL SCI P L A
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method of using a single index to control the quality of traditional Chinese medicine cannot fully reflect the type and quantity of the internal chemical components of traditional Chinese medicine, and then reflect the quality of traditional Chinese medicine. In addition, the method of determining the content of synephrine is relatively complicated

Method used

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  • Fingerprint spectrum of immature bitter orange medicinal material and construction method and application of fingerprint spectrum
  • Fingerprint spectrum of immature bitter orange medicinal material and construction method and application of fingerprint spectrum
  • Fingerprint spectrum of immature bitter orange medicinal material and construction method and application of fingerprint spectrum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Example 1: Establishment and verification of HPLC fingerprints of Citrus aurantium medicinal material

[0057] 1. Instruments and reagents

[0058] Shimadzu (SHIMADZU) LC20A high performance liquid chromatograph, equipped with LC-20AT binary pump, SPD-M20A diode array detector, CTO-20A column thermostat and SIL-20AC autosampler, LCsolution chromatography workstation management software and online degasser.

[0059] Water is pure water; methanol and acetonitrile are chromatographically pure; other reagents are analytically pure.

[0060] The 8 batches of Citrus aurantium medicinal materials were all purchased from genuine medicinal materials in regular pharmacies (attached with test reports according to the Pharmacopoeia).

[0061] 2. Establishment of HPLC fingerprints of Citrus aurantium medicinal material

[0062] 2.1 Preparation of the test solution: Weigh 10 g of the first batch of Citrus aurantium medicinal material, add 100 mL of distilled water to reflux for ...

Embodiment 2

[0078] Example 2: Qualitative identification of characteristic peaks in the HPLC fingerprint of Citrus aurantium medicinal material

[0079] 1. Instruments and reagents: Aglient1100 liquid chromatograph; Aglient6300Ion Trap mass spectrometer; water is pure water; methanol and acetonitrile are chromatographically pure; other reagents are analytically pure; medicinal materials are purchased from regular pharmacies.

[0080] 2. Chromatography and mass spectrometry conditions: Agilent TC-C column packing 18 , the specification is 250mm×4.6mm, 5μm; the mobile phase is acetonitrile-water (containing 0.1% formic acid) gradient elution; the gradient elution conditions are: 0min→20min→45min→60min→75min→77min, acetonitrile 3%→20% →20%→30%→80%→100%; flow rate 1.0mL / min; column temperature 30°C; injection volume 5μL; ion source is ESI, scan in negative ion mode, nebulizer pressure is 40psi, dryer flow rate is 10.0L / min, the ion source temperature is 350°C, and the mass scan range is 20...

Embodiment 3

[0087] Example 3: Application of Standard Fingerprint Spectrum in Identifying Citrus Aurantium Medicinal Material

[0088] 1. Instruments and reagents

[0089] Shimadzu (SHIMADZU) LC20A high performance liquid chromatograph, equipped with LC-20AT binary pump, SPD-M20A diode array detector, CTO-20A column thermostat and SIL-20AC autosampler, LCsolution chromatography workstation management software and online degasser.

[0090] Water is pure water; methanol and acetonitrile are chromatographically pure; other reagents are analytically pure.

[0091] The medicinal materials of Fructus Aurantii to be tested were randomly purchased; the standard sample was the first batch of Fructus Aurantii medicinal materials in Example 1.

[0092] 2. Determination of HPLC fingerprints of Citrus aurantium medicinal material

[0093] 2.1 Preparation of the test solution: Weigh 10 g of Citrus aurantii medicinal material, add 100 mL of distilled water to reflux for extraction twice, each time fo...

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Abstract

The invention belongs to the technical field of pharmaceutical analysis and relates to a fingerprint spectrum of an immature bitter orange medicinal material and a construction method and application of the fingerprint spectrum. Specifically, the invention relates to a high performance liquid chromatography (HPLC) fingerprint spectrum of the immature bitter orange medicinal material and a construction method of the fingerprint spectrum, as well as application of the HPLC fingerprint spectrum and / or a standard fingerprint spectrum of the immature bitter orange medicinal material in identification of the immature bitter orange medicinal material. The method for constructing the HPLC fingerprint spectrum of the immature bitter orange medicinal material specifically comprises the following steps: (1) preparing an immature bitter orange test sample; and (2) performing HPLC analysis. The invention also relates to a method for identifying the immature bitter orange medicinal material. The method is applied to identifying the authenticity and quality of the immature bitter orange medicinal material.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, and relates to a fingerprint of citrus citrus medicinal material, its establishment method and application. Specifically, the present invention relates to a high-performance liquid chromatography (HPLC) fingerprint of Citrus aurantium medicinal material and its establishment method, and the use of HPLC fingerprint and / or standard fingerprint of Citrus aurantium medicinal material in identifying medicinal material of Citrus aurantium. The invention also relates to a method for identifying the quality (whether qualified or not) of the citrus citrus medicinal material. Background technique [0002] Traditional Chinese medicine fingerprint refers to the spectrum of common peaks that can indicate the characteristics of the Chinese medicinal material or Chinese patent medicine obtained after appropriate processing of a certain (or a certain place of origin) Chinese medicinal material or Chinese p...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 乔善义孙磊刘晓晴
Owner INST OF PHARMACOLOGY & TOXICOLOGY ACAD OF MILITARY MEDICAL SCI P L A
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