HPLC detection method for alpinia-cyperus preparations

A detection method and a well-attached technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of non-testing, etc., and achieve the effects of improving safety, comprehensive information reflection, and accurate and reliable measurement results

Active Publication Date: 2016-02-03
CHENGDU UNIV OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] As a compound preparation of traditional Chinese medicine, Liangfu Pill has the characteristics of multi-component, multi-target, multi-level, and overall effect. other ingredients were not tested

Method used

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  • HPLC detection method for alpinia-cyperus preparations
  • HPLC detection method for alpinia-cyperus preparations
  • HPLC detection method for alpinia-cyperus preparations

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Experimental program
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Effect test

Embodiment 1

[0068] The preliminary test of embodiment 1 detection method of the present invention

[0069] Since galangin and kaempferol are quite polar, in the preliminary test, the inventor tried a variety of chromatographic conditions including known literature, but it was difficult to separate galangin from kaempferol. For example:

[0070] With reference to the method in the literature "HPLC method is determined the content of galangin and kaempferol in galanga" (Li Zhiyong etc., Chinese Journal of Traditional Chinese Medicine, the 9th phase of the 25th volume in September, 2010, the 1368-1370 page), below The galangin and kaempferol reference substances were determined in the chromatographic conditions:

[0071] Column: Phenomenex C 18 Chromatographic column (4.6mm×250mm, 5μm)

[0072] Detection wavelength: 360nm;

[0073] Mobile phase: methanol-0.4% phosphoric acid (60:40)

[0074] Volume flow: 1.0mL / min;

[0075] Column temperature: 30°C;

[0076] Injection volume: 10μL;

...

Embodiment 2

[0080] Embodiment 2 detection method of the present invention and methodology investigation

[0081] 1. Preparation of reference solution

[0082] Take an appropriate amount of galangin, kaempferol, cyperenone, citronone, and α-cyperone reference substances, accurately weigh them, place them in a 50mL measuring bottle, dissolve them with chromatographic methanol and dilute to the mark to obtain a mixed control stock solution. Precisely measure 1 mL of the above stock solution, put it in a 10 mL measuring bottle, dissolve it with chromatographic methanol and dilute to the mark to obtain the reference substance solution, the mass concentrations are 0.254, 0.032, 0.051, 0.005, 0.021 mg / mL, respectively.

[0083] 2. Preparation of the test solution

[0084] Take about 1g of Liangfu pill powder, weigh it accurately, put it in a stoppered Erlenmeyer flask, accurately add 25mL of methanol, weigh it, ultrasonically treat it (power 250W, frequency 40kHz) for 30min, let it cool, weigh...

Embodiment 3

[0115] The screening test of embodiment 3 detection method of the present invention

[0116] 1. Screening of detection wavelength

[0117] Under the following chromatographic conditions, compare the wavelengths of 235nm, 242nm, 254nm, 266nm, and 280nm.

[0118] Chromatographic column: Phenomenex C18 chromatographic column (4.6mm×250mm, 5μm);

[0119] Mobile phase: methanol-water;

[0120] Volume flow: 1.0mL / min;

[0121] Column temperature: 30°C;

[0122] Gradient elution program:

[0123]

[0124] result Such as Figure 8-12 shown.

[0125] The results show that at 242nm, each component to be tested has a large ultraviolet absorption, so 242nm is selected as the detection wavelength.

[0126] 2. Screening of mobile phase and gradient elution program

[0127] Various mobile phases and gradient elution programs such as methanol-water, methanol-0.2% phosphoric acid, acetonitrile-0.2% phosphoric acid, etc. were investigated, and the conditions were as follows:

[01...

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Abstract

The invention discloses an HPLC detection method for alpinia-cyperus preparations. The HPLC method is used for simultaneous determination of the contents of 5 components, namely galangin, kaempferide, sweet ketene, nootkatone and alpha-cyperone, in the alpinia-cyperus preparations. The HPLC method comprises the following steps: (1) establishing a standard curve of galangin, kaempferide, sweet ketene, nootkatone and alpha-cyperone; (2) determining the contents of galangin, kaempferide, sweet ketene, nootkatone and alpha-cyperone in a sample to be detected. According to the HPLC detection method provided by the invention, various components in the alpinia-cyperus preparations can be determined simultaneously. The HPLC method is high in specificity, can comprehensively reflect information, is simple and convenient, quick and accurate, and is accurate and reliable in determination result, so that the quality of the alpinia-cyperus preparations can be effectively monitored, and the medicine safety is improved.

Description

technical field [0001] The invention relates to the technical field of drug quality control methods, in particular to a quality detection method for liangfu preparations. Background technique [0002] Liangfu pills were first recorded in "Liangfang Jixiong" written by Xie Yuanqing in the Qing Dynasty. The representative preparation of TCM has a history of nearly a thousand years in clinical application of traditional Chinese medicine. As a typical traditional Chinese medicine compound preparation, Liangfu Pills has a fixed medicinal composition, simple preparation process, remarkable clinical curative effect and great potential for development. [0003] As a compound preparation of traditional Chinese medicine, Liangfu Pill has the characteristics of multi-component, multi-target, multi-level, and overall effect. Other ingredients were not tested. [0004] Therefore, there is a need for a detection method that can comprehensively reflect the quality of the preparations of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 卢君蓉李文兵王世宇傅超美傅舒季宁平严鑫
Owner CHENGDU UNIV OF TRADITIONAL CHINESE MEDICINE
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