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Preparation method and application of nigella damascena saponin A

A technology of herbasaponin and nigella nigella, which is applied in the field of preparation of nigella saponin A, can solve the problems of limited preparation scale, low yield, complicated separation and preparation process steps, etc., and achieve automation, production feasibility and high purity , The effect of simplifying the purification process burden

Inactive Publication Date: 2016-04-20
SUZHOU QIUSHI HERBAL HEALTH TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Existing literature research on Semen Nigella focuses on the separation and identification of this type of saponins. Generally, complex processes such as alcohol extraction, macroporous resin purification, silica gel and reversed-phase silica gel multiple column chromatography purification are used. The separation and preparation process steps Complex, low yield, mainly limited to the scale of laboratory preparation

Method used

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  • Preparation method and application of nigella damascena saponin A
  • Preparation method and application of nigella damascena saponin A
  • Preparation method and application of nigella damascena saponin A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The preparation of embodiment 1 nigella saponin A

[0020] The medicinal material of Nigella nigella was purchased from Urumqi, Xinjiang Uygur Autonomous Region (batch number: NG20121025), and it was identified as the dried mature seeds of Nigella glandulifera Freynet Sint, a plant of Ranunculaceae.

[0021] Nigella saponin A content was determined by HPLC, chromatographic conditions: AgilentTC-C18 chromatographic column (250mm×4.6mm, 5 μm); ELSD detection; mobile phase was acetonitrile-water (32:68) isocratic elution for 20min; flow rate 1.0mL / min; column temperature 40°C; injection volume 20 μL. The preparation process of the macroporous resin was carried out with reference to Luan Ming’s report [Chinese Journal of Pharmaceutical Sciences, 2014, 49(12): 1014-1017].

[0022] (1) Take 10kg of black cumin medicinal material after oil extraction, add 10 times the amount of 70% ethanol to reflux extraction for 3 times, each time for 1h; combine the filtrate, recover unde...

Embodiment 2

[0024] The preparation of embodiment 2 nigella saponin A

[0025] Get 2L of Nigella saponins concentrated solution obtained in Example 1 (1), add 500ml of methanol to dilute, filter, put on a Daisogel RP-18 column (80-120 μm, column volume 4L) medium pressure preparative chromatography, 45% → 55% methanol gradient The elution time is 120min, the elution flow rate is 300mL / min, and the detection wavelength is 210nm. The pooled fractions of nigural saponin A were detected by HPLC, concentrated under reduced pressure, and vacuum-dried at 50° C. to obtain 31 g of nigural saponin A (content 91.4%).

Embodiment 3

[0026] The preparation of embodiment 3 nigella saponin A

[0027] (1) Take 10kg of black cumin medicinal material after oil extraction, add 15 times the amount of 50% ethanol to reflux and extract twice, each time for 1.5h; combine the filtrates, concentrate under reduced pressure until there is no alcohol smell, dilute with water to 40L, filter, and put on HPD450 macroporous resin chromatography column (column volume 30L / BV), first elute 6BV with water, then elute 4BV with 60% ethanol, collect 60% ethanol eluate, concentrate under reduced pressure until no alcohol smell, dilute with water to 50L , first filter with an ultrafiltration ceramic membrane (0.05 μm pore size), collect 40 L of permeate, and then filter with a nanofiltration organic membrane (molecular weight cut-off 200 Da) to collect 5 L of Nigella total saponins concentrate. The solid content in the concentrated solution was determined to be 62g / L, and the content of nigosaponin A was 76.7%.

[0028] (2) Take 1 L...

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Abstract

The invention discloses a preparation method of nigella damascena saponin A. The preparation method comprises the following steps: selecting nigella damascena plant seeds; extracting by adopting an ethanol solution; refining by further adopting macroporous resin and concentrating to obtain a concentrated solution of nigella damascena total saponins; separating the concentrated solution by adopting a pressurized preparation chromatographic system, taking C18 modified silica gel in the particle size range of 20 to 120 mu m as a filler, and taking 40 to 60 percent methyl alcohol as a moving phase; collecting, concentrating and drying a fraction which contains the nigella damascena saponin A to obtain the finished nigella damascena saponin A with the purity of greater than 90 percent. The product prepared by the invention is high in purity, simple in process and high in operability, and facilitates the implementation of industrialized amplification. The nigella damascena saponin A disclosed by the invention has definite effects of resisting colon cancer and resisting inflammation, so that the nigella damascena saponin A can be applied to related medicine or healthcare food with tumor resisting and inflammation resisting functions.

Description

technical field [0001] The invention relates to a preparation method of nigella saponin A, and also relates to the application of the compound in anti-tumor and anti-inflammatory effects, belonging to the field of health food and biomedicine. technical background [0002] Plants of the genus Nigella (Ranunculaceae) are distributed in the Mediterranean Sea, West Asia, Central Asia, and Xinjiang, China. Aggregation, anti-oxidation, anti-tumor, liver protection, lipid-lowering, hypoglycemic and other pharmacological activities, often used for chest tightness, gas foot, breast swelling, reduced milk, tinnitus, hot shower, stone shower, amenorrhea and other diseases. Black cumin contains 30-35% oil, which is a functional food commonly used by Uighurs; in addition, black cumin is also rich in flavonoids, saponins, alkaloids and other biologically active substances. In recent years, the saponins contained in Nigella cumin have certain anti-tumor activity in vitro, so their researc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J63/00A61P35/00A61P29/00A23L33/105A23L33/125
CPCC07J63/008A23V2002/00A61K31/704A23V2200/308A23V2250/21
Inventor 田景奎张琳李守信周生海刘江云
Owner SUZHOU QIUSHI HERBAL HEALTH TECH CO LTD