Simultaneous preparation and detection method of gallic acid and gallicin in toona sinensis leaves

A technology of methyl gallate and gallic acid, applied in the field of traditional Chinese medicine, can solve the problems of poor reliability, high cost, complicated operation and the like, and achieve the effects of simple operation, high reliability, and low consumption of time and reagents

Inactive Publication Date: 2013-04-24
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The object of the present invention is to overcome the deficiencies such as prior art can not carry out simultaneous preparation to gallic acid and its methyl ester, complex operation, high cost, poor reliability of analysis, difficult application, etc. Simultaneous preparation of two plant-derived antioxidants gallic acid and methyl gallate, and a method for determining the content of these two components in Chinese toon leaf medicinal materials

Method used

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  • Simultaneous preparation and detection method of gallic acid and gallicin in toona sinensis leaves
  • Simultaneous preparation and detection method of gallic acid and gallicin in toona sinensis leaves
  • Simultaneous preparation and detection method of gallic acid and gallicin in toona sinensis leaves

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preparation Embodiment 1

[0041] 1kg of mellow leaf fine powder is extracted twice with 5L of 85% ethanol by ultrasonic, each time for 1 hour, and the extracts are combined, 50 o Recover the solvent under reduced pressure below C to obtain the extract; add 6 times the amount of water to suspend, extract 3 times with an equal amount of water-saturated n-butanol, combine the extracts, recover the solvent under reduced pressure, and dry-load the obtained n-butanol extract Loaded into a silica gel column for separation, the mass ratio of the extract to silica gel was 1:50, and the volume ratio of dichloromethane-methanol-water-formic acid was 100:10:1:0.3. : 1.5 (g / mL) to collect a part of the effluent, collect the 6th to 7th part of the effluent, combine, recover the solvent under reduced pressure, and obtain the preliminary purified product; the preliminary purified product: methanol in a ratio of 1:30 (g / mL ) dissolved, and the solution was loaded into a preparative high-performance liquid chromatograph...

preparation Embodiment 2

[0043] 100g of mellow leaf fine powder was extracted 3 times with 700mL of 90% ethanol ultrasonically, each time for 1.5 hours, and the extracts were combined, 50 o Recover the solvent under reduced pressure below C to obtain the extract; add 6 times the amount of water to suspend, extract 3 times with an equal amount of water-saturated n-butanol, combine the extracts, recover the solvent under reduced pressure, and dry-load the obtained n-butanol extract Loaded into a silica gel column for separation, the mass ratio of the extract to silica gel was 1:70, and the volume ratio of dichloromethane-methanol-water-formic acid was 100:12:2:1. : 1.2 (g / mL) to collect a part of the effluent, collect the 6th to 8th part of the effluent, combine, recover the solvent under reduced pressure, and obtain the preliminary purified product; the preliminary purified product: methanol in a ratio of 1:30 (g / mL ) dissolved, and the solution was loaded into a preparative high-performance liquid chr...

preparation Embodiment 3

[0045] 100g of mellow leaf fine powder is extracted 3 times with 90% ethanol 600mL ultrasonically, each time for 1.5 hours, and the extracts are combined, 50 o Recover the solvent under reduced pressure below C to obtain the extract; add 6 times the amount of water to suspend, extract 3 times with an equal amount of water-saturated n-butanol, combine the extracts, recover the solvent under reduced pressure, and dry-load the obtained n-butanol extract Loaded on a silica gel column for separation, the mass ratio of the extract to silica gel was 1:70, and the volume ratio of dichloromethane-methanol-water-formic acid was 100:10:3:3 for isocratic elution, and the silica gel: fraction volume was 1 : 1 (g / mL) to collect an effluent, collect the 5th to 6th effluent, combine, and recover the solvent under reduced pressure to obtain a preliminary purified product; the preliminary purified product: methanol in a ratio of 1:50 (g / mL ) for dissolution, and the solution was loaded into a p...

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Abstract

The invention provides a simultaneous preparation and detection method of gallic acid and gallicin in toona sinensis leaves, belonging to the technical field of traditional Chinese medicine. Through the adopted preparation method, the gallic acid and the gallicin can be simultaneously obtained from the traditional Chinese medicine toona sinensis leaves by means of drawing, extracting and secondary column chromatography, so that the use of various column chromatography padding and repeated column chromatography can be avoided, and the simultaneous preparation method is easy and simple to operate, and low in time and reagent consumption; and in the adopted detection method, the high-efficiency liquid phase chromatographic instrument normally prepared in a laboratory is used, various methodology indexes, i.e., the separation degree, the veracity, the reproducibility, the stability and the like meet the content detecting requirement, the simultaneous preparation method is high in reliability, the method can be used for analyzing the content of the gallic acid and the gallicin in the toona sinensis leaves medicinal materials with different sources and batches, and the requirements of the pharmacological activity test and the normal quality control of the traditional Chinese medicine can be met.

Description

[0001] technical field [0002] The invention relates to the simultaneous preparation and quantitative detection of gallic acid and methyl gallate, two antioxidant active substances in Toona sinensis leaves, by using high-performance liquid chromatography technology, and belongs to the technical field of traditional Chinese medicines. Background technique [0003] Toona sinensis (Meliaceae tree) Toona sinensis A. Juss. Roemer) is widely distributed throughout Asia, especially in China and India. The fresh young leaves (Chinese Toon) harvested in spring are one of the local people's favorite seasonal vegetables. In addition, Toonea Sinensis Folium is the dry leaves of the plant, which is a traditional Chinese medicine with detoxification and anti-inflammatory effects. It is mainly used to treat bad breath, vomiting, dysentery, loss of appetite, enteritis and pruritus. No side effects have been observed so far. [0004] On the one hand, because antioxidants can effective...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C65/03C07C51/47C07C69/88C07C67/56G01N30/02G01N30/06
Inventor 杨欢刘丹沈玉萍余筱洁周存山夏国华江晓萍
Owner JIANGSU UNIV
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