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Method for preparing chemical reference substances used in chromatographic separation of Oxytropis based on parallel separation mode

A separation mode and technology for separating Oxytropis, applied in chemical instruments and methods, medical preparations containing active ingredients, organic chemistry, etc., can solve the problem of not systematically and deeply studying the mechanism of action of active substances in Oxytropis and failing to meet the requirements of Oxytropis. Quality control requirements for new drug creation, restrictions on the development and research of Oxytropis medicinal materials, etc., to achieve the effects of rapid separation and preparation, increased chemical production, and good anticancer activity

Active Publication Date: 2017-02-01
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] At present, scholars from various countries have isolated more than 140 compounds from more than 20 kinds of medicinal plants of the genus Oxytropis, most of which are flavonoids, triterpenoids and alkaloids. There is no systematic and in-depth study on the active substances in Oxytropis. Mechanism of action, only preliminary pharmacological activity studies have been conducted
At the same time, it is also impossible to stably obtain chemical reference substances with a purity of more than 98%, which cannot meet the quality control requirements for the creation of new drugs and related preparations of Oxytropis chinensis, thus restricting the medicinal development and research of Oxytropis chinensis medicinal materials

Method used

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  • Method for preparing chemical reference substances used in chromatographic separation of Oxytropis based on parallel separation mode
  • Method for preparing chemical reference substances used in chromatographic separation of Oxytropis based on parallel separation mode
  • Method for preparing chemical reference substances used in chromatographic separation of Oxytropis based on parallel separation mode

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Experimental program
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Effect test

Embodiment 1

[0044] Embodiment 1 The method for preparing a chromatographically separated chemical reference substance in Oxytropis based on a parallel separation mode comprises the following steps:

[0045] ⑴ Preparation of Oxytropis extractum:

[0046] The Oxytropis falciparum is ultrasonically extracted with 5% ethanol to obtain an extract; the extract is concentrated under reduced pressure to obtain the Oxytropis extract extract.

[0047] in:

[0048] The conditions of ultrasonic extraction were that the ratio of solid to liquid was 1 g: 5 mL, the extraction temperature was 50 °C, the extraction times were 1 time, each time 1 h, and the ultrasonic power was 1 KW.

[0049] The conditions for concentration under reduced pressure refer to a vacuum degree of 0.07 MPa and a water bath temperature of 65°C.

[0050] ⑵Extraction:

[0051] After dissolving the Oxytropis extract extract in deionized water with 1 times its mass, it was extracted with petroleum ether and ethyl acetate in sequen...

Embodiment 2

[0062] Embodiment 2 The method for preparing a chromatographically separated chemical reference substance in Oxytropis based on a parallel separation mode comprises the following steps:

[0063] ⑴ Preparation of Oxytropis extractum:

[0064] The Oxytropis gansuensis is ultrasonically extracted with ethanol with a volume concentration of 95% to obtain an extract; the extract is concentrated under reduced pressure to obtain the Oxytropis extract extract.

[0065] in:

[0066] The conditions of ultrasonic extraction were that the ratio of solid to liquid was 1 g: 30 mL, the extraction temperature was 95°C, the extraction times were 4 times, each time 4 h, and the ultrasonic power was 100KW.

[0067] The conditions for concentration under reduced pressure refer to a vacuum degree of 0.05 MPa and a water bath temperature of 70°C.

[0068] ⑵Extraction:

[0069] The Oxytropis extract extract was dissolved in deionized water 10 times its mass, and then extracted with petroleum ethe...

Embodiment 3

[0080] Embodiment 3 The method for preparing a chromatographically separated chemical reference substance in Oxytropis based on a parallel separation mode comprises the following steps:

[0081] ⑴ Preparation of Oxytropis extractum:

[0082] Ultrasonic extraction of Oxytropis multi-leaf with methanol with a volume concentration of 5% was used to obtain an extract; the extract was concentrated under reduced pressure to obtain Oxytropis extract.

[0083] in:

[0084] The conditions of ultrasonic extraction are that the ratio of solid to liquid is 1 g: 30 mL, the extraction temperature is 75°C, the extraction times are 2 times, each time 2h, and the ultrasonic power is 70KW.

[0085] The conditions for concentration under reduced pressure refer to a vacuum degree of 0.08 MPa and a water bath temperature of 75°C.

[0086] ⑵Extraction:

[0087] The Oxytropis extract extract was dissolved in deionized water 10 times its mass, and then extracted with petroleum ether and ethyl acet...

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Abstract

The invention relates to a method for preparing chemical reference substances used in chromatographic separation of Oxytropis based on a parallel separation mode. The method comprises the following steps: (1) preparing Oxytropis extract: subjecting Oxytropis to ultrasonic extraction and pressure-reduced concentration so as to obtain the Oxytropis extract; (2) carrying out extraction: subjecting the Oxytropis extract to dissolving and extraction so as to obtain a petroleum ether part, an ethyl acetate part and a water part, respectively; (3) drying the water part to a constant weight so as to obtain dried powder of the water part; and (4) dissolving the dried powder of the water part, then carrying out separation by using a preparative chromatographic device with a parallel separation mode so as to obtain two compounds meeting requirements of chemical reference substances and having purity of more than 98%, i.e., maltol-3-o-beta-D-glucoside and tryptophan. The method provided by the invention has the advantages of simple process, high repeatability and high recovery rate; and the two obtained compounds have good anticancer activity.

Description

technical field [0001] The invention relates to a preparation method of a chemical reference substance, in particular to a method for preparing a chromatographically separated chemical reference substance in Oxytropis chinensis based on a parallel separation mode. Background technique [0002] Plants of the genus Oxytropis (Oxytropis D.C.) belong to the Fabaceae Papilionaceae. This genus is a perennial herb, semi-shrub or shrub. There are more than 300 species in the world, and there are 131 species of Oxytropis (medicinal plants) in my country. There are more than 20 species), which are distributed in Gansu, Qinghai, Inner Mongolia, Sichuan, Tibet and other places. The medicinal plants of the genus Oxytropis were recorded in the 1977 edition of the Chinese Pharmacopoeia. It is widely distributed in my country and is often used in compound prescriptions of Tibetan and Mongolian medicines. [0003] Oxytropis falcate Bunge (Tibetan medicine name is Oxytropis D.C.) is a perenni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08C07D209/20A61K31/7048A61K31/405A61P29/00A61P7/04A61P19/00A61P31/08A61P31/04A61P31/16A61P11/04A61P11/00A61P35/00
CPCA61K31/405A61K31/7048C07D209/20C07H1/08C07H17/04A61K2300/00
Inventor 陈晨陈涛李玉林王环谭亮赵景阳
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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