HPLC (High Performance Liquid Chromatography) method for simultaneously determining content of six organic acids in pinellia ternata

A technology of organic acid and pinellia, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of good reproducibility, high accuracy and sensitivity

Inactive Publication Date: 2015-05-06
CHONGQING MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Overcome the defects of the existing potentiometric titration method for the determination of total organic acids in Pinellia medicinal materials

Method used

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  • HPLC (High Performance Liquid Chromatography) method for simultaneously determining content of six organic acids in pinellia ternata
  • HPLC (High Performance Liquid Chromatography) method for simultaneously determining content of six organic acids in pinellia ternata
  • HPLC (High Performance Liquid Chromatography) method for simultaneously determining content of six organic acids in pinellia ternata

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 1 Instruments and reagents:

[0015] Shimadzu LC-15C liquid chromatograph, LabSolutions LC workstation (Shimadzu, Japan); AG135 electronic analytical balance (Mettler toledo, Switzerland); KQ2200B ultrasonic cleaner (Kunshan Ultrasonic Instrument Co., Ltd.); RE-52AA Rotary evaporator (Shanghai Yarong Biochemical Instrument Factory); PHS-3C pH meter (Shanghai Yidian Scientific Instrument Co., Ltd.);

[0016] 10 pinellia medicinal materials from different origins were identified as dried tubers of Pinellia ternata (Thunb.) Breit by the quality inspection department of Chongqing Taiji Group; oxalic acid reference substance (National Institute for Food and Drug Control, batch number: 100328-201010) ; Formic acid (content ≥ 98.0%, Chongqing Chuandong Chemical Co., Ltd.); Acetic acid (content ≥ 99.5%, Chongqing Chuandong Chemical Co., Ltd.); Citric acid reference substance (China Institute for Food and Drug Control, batch number: 111598-200904); Malic acid reference substanc...

Embodiment 2

[0040] 2.3 Preparation of sample solution: Weigh 2.0g of dried pinellia herb powder, weigh it accurately, add 40mL of water, weigh it, ultrasonically, 300W, 25kHz, extract twice, each time for 2h, put it to room temperature, and weigh again , make up for the lost weight with water, filter the extract with a sand core Bush funnel, put the combined filtrate in a 100mL volumetric flask, add water to volume, accurately measure 20mL of the filtrate in a small beaker, add ammonia water dropwise to adjust the pH to 11.5, and use the extract Extract 3 times with 3 times the amount of ethyl acetate, collect the alkaline water, add dropwise phosphoric acid to adjust the pH to 2.0, extract 5 times with 3 times the amount of ethyl acetate, collect the ethyl acetate, dry it by rotary evaporation, add ultra-pure Dissolve in water and dilute to 25mL, filter through a 0.22μm filter membrane, and take the subsequent filtrate, which is the sample solution.

[0041] 2.5 Precision test: The RSDs ...

Embodiment 3

[0046] 2.3 Preparation of sample solution: Weigh 2.0g of dried pinellia herb powder, weigh it accurately, add 40mL of water, weigh it, ultrasonically, 300W, 25kHz, extract twice, each time for 2h, put it to room temperature, and weigh again , make up the lost weight with water, filter the extract with a sand core Bush funnel, put the combined filtrate in a 100mL volumetric flask, add water to make up the volume, accurately measure 20mL of the filtrate in a small beaker, add ammonia water dropwise to adjust the pH to 12.0, and use the extract Extract 3 times with 3 times the amount of ethyl acetate, collect the alkaline water, add dropwise phosphoric acid to adjust the pH to 2.0, extract 5 times with 3 times the amount of ethyl acetate, collect the ethyl acetate, dry it by rotary evaporation, add ultra-pure Dissolve in water and dilute to 25mL, filter through a 0.22μm filter membrane, and take the subsequent filtrate, which is the sample solution.

[0047] 2.5 Precision test: T...

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Abstract

The invention relates to an HPLC (High Performance Liquid Chromatography) method for simultaneously determining content of six organic acids in pinellia ternata. The method comprises the following steps: (1) preparing a sample solution; (2) preparing a comparison product solution; (3) determining by a high performance liquid chromatography: taking the comparison product solution and the sample solution and carrying out determination analysis under following chromatographic conditions: a chromatographic column is GL InterSustain-C18 (4.6mm*250mm, 5 microns), and a mobile phase is a phosphoric acid adjusted 0.03mol/L (NH4)H2PO4 buffering solution with the pH value of 2.0 and methanol; and the volume ratio is 97 to 3, the flow speed is 0.8mL/min, the column temperature is 30 DEG C and the detection wavelength is 210nm. Under the conditions of the method, oxalic acid, formic acid, malic acid, acetic acid, citric acid and succinic acid in pinellia ternata are effectively separated, and methodological results meet the analysis determination requirements. Compared with the traditional potentiometric titration method, the measurement for content of total organic acids is clear and objective by virtue of the HPLC method disclosed by the invention, and the content of the six organic acids in pinellia ternata can be effectively and rapidly determined and the quality of pinellia ternata can be comprehensively and accurately controlled.

Description

technical field [0001] The invention relates to a traditional Chinese medicine determination method, in particular to a method for simultaneously determining the contents of six kinds of organic acids in pinellia pinellia by using HPLC. Background technique [0002] Pinellia is the dry tuber of Pinellia ternata (thunb.) Breit., another name for Pinellia ternata (thunb.) Breit. Sichuan, Hubei, Henan and Guizhou. Spicy and warm in nature, it has the effects of drying dampness and resolving phlegm, reducing adverse reactions and relieving vomiting, dispelling swelling and dispelling stagnation, and is clinically used for diseases such as excessive phlegm and cough, dyspnea with phlegm and retention, vertigo due to wind-phlegm, vomiting and regurgitation, and fullness in the chest cavity. a lot of uses. Pinellia contains a variety of chemical components, mainly including organic acids, alkaloids, pinellia proteins and phenols. A study reported that the relationship between th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 何丹张景勍孙全杨林
Owner CHONGQING MEDICAL UNIVERSITY
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