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Detection method for HPLC characteristic atlas of Liang Di decoction

A detection method and characteristic map technology, applied in the field of characteristic map detection, can solve the problems of complex chemical composition and difficult quality control of soup

Active Publication Date: 2019-11-05
SHAN DONG DONG E E JIAO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that the chemical composition of Liangdi soup is complex, and the quality control is difficult
Up to now, there is no literature report on Liangdi Decoction quality detection and control methods, therefore, it is urgent and critical to establish Liangdi Decoction quality control methods

Method used

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  • Detection method for HPLC characteristic atlas of Liang Di decoction
  • Detection method for HPLC characteristic atlas of Liang Di decoction
  • Detection method for HPLC characteristic atlas of Liang Di decoction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: preparation of Liangdi Decoction

[0032] Wine Rehmannia 37.3g, Scrophulariaceae 37.3g, Wine White Peony 18.6g, Ophiopogon japonicus 18.6g, Digupi 11.2g, Ejiao 11.2g

[0033] For the above six flavors, take wine rehmannia glutinosa, scrophulariaceae and other five flavors except donkey-hide gelatin, soak in water for 40 minutes, cover and cook twice, add 7 times the amount of water for the first time, and cook for 30 minutes; add 5 times the amount of water for the second time, fry Boil for 20 minutes; filter the decoction, combine and concentrate the filtrates to about 500ml, add donkey-hide gelatin to melt, and obtain a standard decoction; the standard decoction is concentrated at low temperature and reduced pressure to about 250ml, freeze-dried into a lyophilized powder, and obtained.

Embodiment 2

[0034] Example 2: Establishment of Liangdi Tang characteristic map method

[0035] 1. Instruments and reagents

[0036] Instrument: Shimadzu LC-20AT high performance liquid chromatography (DGU-20A5 online degassing system, LC-20AT series double plunger pump, SIL-20A autosampler, CTO-20AC column thermostat, SPD-M20A diode array detector); high performance liquid chromatography (U.S., Agilent 1290 series, Agilent company)-quadrupole time-of-flight mass spectrometry (U.S.A., Agilent 6540series, Agilent company); Sartorious M-power 1 / 10,000 electronic balance and Sartorious TE212-L 1% electronic balance (Sartorius Scientific Instruments (Beijing) Co., Ltd.), XS105DU 1 / 100,000 electronic balance (Switzerland, Mettler-Toledo); KQ-500E ultrasonic cleaner ( Kunshan Ultrasonic Instrument Co., Ltd.); DK-98-IIA electric heating constant temperature water bath (Tianjin Test Instrument Co., Ltd.).

[0037] Reference substances and reagents: standard paeoniflorin (batch number: 110736-201...

Embodiment 3

[0080] Example 3: Liangdi Decoction Feature Map

[0081] Chromatographic conditions and system suitability test Octadecylsilane bonded silica gel was used as filler (ThermoHypersil GOLDTM aQ chromatographic column, column length is 25cm, inner diameter is 4.6mm, particle size is 5μm); methanol is used as mobile phase A, and 0.05% phosphoric acid solution is the mobile phase B, and carries out gradient elution as specified in the table below; the flow rate is 1ml / min; the detection wavelength is 254nm, 210nm; the column temperature is 25°C. The number of theoretical plates calculated based on the peak of paeoniflorin is not less than 3000.

[0082]

[0083] Preparation of reference solution Take appropriate amount of reference substances of paeoniflorin and harpagoside, weigh them accurately, add methanol to make a mixed solution containing 180 μg of paeoniflorin and 20 μg of harpagoside per 1 ml.

[0084] Preparation of the test solution Take this product and grind it fine...

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Abstract

The invention discloses a detection method for an HPLC characteristic atlas of a Liang Di decoction. The method is characterized by comprising the following steps that (1) a tested object solution isprepared by taking a preparation of the Liang Di decoction to be detected; (2) a contrast solution is prepared by taking paeoniflorin and harpagoside; and (3) a contrast characteristic atlas is made by absorbing the tested object solution and the contrast solution and injecting the solutions into a high efficiency liquid chromatograph, generating the contrast characteristic atlas according to atlas obtained by measuring N batches of tested objects, and calculating relative retention time with other shared peaks by taking retention time of a chromatographic peak of the reference object as reference. The method is higher in precision, satiability and repeatability, and can be used to comprehensively and effectively control the quality of the Liang Di decoction.

Description

technical field [0001] The invention belongs to the technical field of drug quality control, in particular, the invention relates to a detection method and application of a characteristic map of Liangdi Decoction. Background technique [0002] Liangdi Decoction comes from the book "Fu Qingzhu Gynecology" written by Fu Shan (word Qingzhu) in the late Ming and early Qing Dynasties. It is widely used and is often used in gynecology. The main functions of Liangdi Decoction are nourishing yin and clearing heat, cooling blood and regulating menstruation. It is mainly used to treat early menstruation, less menstrual flow, prolonged menstruation and dysfunctional uterine bleeding caused by yin deficiency and internal heat. [0003] Due to the large number of raw materials and complex components of traditional Chinese medicine compound recipes, it is difficult to control the quality. The characteristic map can more comprehensively reflect the type and overall characteristics of the...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/36
CPCG01N30/02G01N30/06G01N30/14G01N30/36G01N2030/047G01N2030/146
Inventor 孔令梅刘海滨张淹周祥山张路李士栋王春艳齐晓丹
Owner SHAN DONG DONG E E JIAO
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