Raw fleece-flower root HPLC fingerprint detection method

Abstract

The invention discloses a raw fleece-flower root HPLC fingerprint detection method. The detection method comprises the following steps: (1) preparing a control substance solution; (2) preparing a reference substance solution; (3) establishing a control fingerprint; (4) preparing a test article solution; (5) detecting the test article solution. The obtained fingerprint has the advantages that there are many peaks, the resolution and repeatability are good, the precision is high, and the quality of raw fleece-flower root can be effectively monitored. By using the extraction method and chromatogram conditions of provided fingerprint detection method, contents of 16 components of raw fleece-flower root can be measured, and thus the quality of raw fleece-flower root can be monitored from more aspects.

Description

technical field

[0001] The invention relates to the technical field of drug quality control methods, in particular to an HPLC fingerprint detection method for raw Polygonum multiflorum. Background technique

[0002] Polygonum multiflorum is the dry tuber root of Polygonum multiflorum Thunb., which is flat in nature, sweet in taste, bitter in taste, and has the effects of detoxifying, eliminating carbuncle, cutting malaria, and laxative; it is commonly used traditional Chinese medicine. It is widely distributed throughout the country and is mainly produced in Henan, Hubei, Guangxi, Guangdong, Guizhou, Sichuan and other places.

[0003] The stilbene glycosides and anthraquinones in Polygonum multiflorum are their representative active ingredients. Among them, stilbene glycosides have significant neuroprotective effects; anthraquinone components have anti-inflammatory, anti-pathogenic microorganisms, anti-tumor, diuretic, and liver-protecting effects, among which emodin has a...

Examples

Embodiment 1

[0053] The screening of embodiment 1 experimental conditions

[0054] 1. Screening of mobile phase conditions

[0055] Under the same sample injection conditions of Radix Polygoni Multiflori, 0.1% formic acid water and acetonitrile were used as pump A and pump B of the eluting mobile phase, and the gradient elution conditions were carried out with different volume ratios (v / v) of A and B in different time periods Screening, gradient elution procedures are shown in Table 2, and the corresponding fingerprints of Radix Polygoni Multiflori are obtained in Table 2. figure 1 (A-F), by figure 1 It can be seen that figure 1 A basically failed to separate; figure 1 B, C, D part of the time point map can not be separated; figure 1 In part of the period of time in E, the baseline drifts seriously, figure 1 In F, each component is well separated, and the baseline is basically stable, so the gradient elution condition is set as the fingerprint analysis condition of Radix Polygon...

Embodiment 2

[0066] Embodiment 2 The method of the present invention and its methodology verification

[0067] 1 Preparation of sample solution

[0068] 25 batches of raw Shouwu commercially available were beaten into coarse powder for later use. Accurately weigh 0.25 g of each coarse powder, put it in a stoppered Erlenmeyer flask, add 20 times the amount of 50% ethanol aqueous solution, soak for 30 minutes, ultrasonically extract at 40°C for 60 minutes, and dilute to 5 mL. Filter through a 0.45 μm microporous membrane, and take the subsequent filtrate for injection.

[0069] 2.2 Preparation of reference solution

[0070] Accurately weigh the reference substances gallic acid and proanthocyanidin B 1 , catechin, gallic acid ester, aloe-emodin glycoside, polydatin, stilbene glycoside, rhein, resveratrol, emodin glycoside, emodin methyl ether glycoside, aloe-emodin, rhein, chrysophanol , emodin, and emodin methyl ether reference substances in a 10mL volumetric flask, set the volume to the...

technical field

[0001] The invention relates to the technical field of drug quality control methods, in particular to an HPLC fingerprint detection method for raw Polygonum multiflorum. Background technique

[0002] Polygonum multiflorum is the dry tuber root of Polygonum multiflorum Thunb., which is flat in nature, sweet in taste, bitter in taste, and has the effects of detoxifying, eliminating carbuncle, cutting malaria, and laxative; it is commonly used traditional Chinese medicine. It is widely distributed throughout the country and is mainly produced in Henan, Hubei, Guangxi, Guangdong, Guizhou, Sichuan and other places.

[0003] The stilbene glycosides and anthraquinones in Polygonum multiflorum are their representative active ingredients. Among them, stilbene glycosides have significant neuroprotective effects; anthraquinone components have anti-inflammatory, anti-pathogenic microorganisms, anti-tumor, diuretic, and liver-protecting effects, among which emodin has a...

Examples

Embodiment 1

[0053] The screening of embodiment 1 experimental conditions

[0054] 1. Screening of mobile phase conditions

[0055] Under the same sample injection conditions of Radix Polygoni Multiflori, 0.1% formic acid water and acetonitrile were used as pump A and pump B of the eluting mobile phase, and the gradient elution conditions were carried out with different volume ratios (v / v) of A and B in different time periods Screening, gradient elution procedures are shown in Table 2, and the corresponding fingerprints of Radix Polygoni Multiflori are obtained in Table 2. figure 1 (A-F), by figure 1 It can be seen that figure 1 A basically failed to separate; figure 1 B, C, D part of the time point map can not be separated; figure 1 In part of the period of time in E, the baseline drifts seriously, figure 1 In F, each component is well separated, and the baseline is basically stable, so the gradient elution condition is set as the fingerprint analysis condition of Radix Polygon...

Embodiment 2

[0066] Embodiment 2 The method of the present invention and its methodology verification

[0067] 1 Preparation of sample solution

[0068] 25 batches of raw Shouwu commercially available were beaten into coarse powder for later use. Accurately weigh 0.25 g of each coarse powder, put it in a stoppered Erlenmeyer flask, add 20 times the amount of 50% ethanol aqueous solution, soak for 30 minutes, ultrasonically extract at 40°C for 60 minutes, and dilute to 5 mL. Filter through a 0.45 μm microporous membrane, and take the subsequent filtrate for injection.

[0069] 2.2 Preparation of reference solution

[0070] Accurately weigh the reference substances gallic acid and proanthocyanidin B 1 , catechin, gallic acid ester, aloe-emodin glycoside, polydatin, stilbene glycoside, rhein, resveratrol, emodin glycoside, emodin methyl ether glycoside, aloe-emodin, rhein, chrysophanol , emodin, and emodin methyl ether reference substances in a 10mL volumetric flask, set the volume to the...

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