A method for preparing crocin-I by high-speed countercurrent chromatography

A technology of high-speed countercurrent chromatography and crocin, which is applied in the field of preparing crocin-I by high-speed countercurrent chromatography, can solve the problems of complex operation and small preparation volume, achieve large separation volume, fast separation speed, and sample lossless effect

Inactive Publication Date: 2011-12-14
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing methods for separating high-content crocin-I are generally silica gel column chromatography and preparative liquid phase. These methods are complicated to operate and have a small amount of preparation

Method used

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  • A method for preparing crocin-I by high-speed countercurrent chromatography

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Experimental program
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Effect test

Embodiment 1

[0016] Take ethyl acetate, ethanol, and water, mix them in a ratio of 7:4:5, let them stand in a separatory funnel for 12 hours, and separate the upper and lower phases. Take the upper phase and fill the high-speed countercurrent chromatographic column, turn the main engine at a speed of 700rpm, pump the lower phase into the mobile phase, and when the mobile phase flows out, adjust the flow rate to 4ml / min, and take the mobile phase to dissolve gardenia yellow with a color value of 400 Pigment 1g, injected by the injection valve, detected by SP-200 ultraviolet detector, collected the target components according to the spectrum, concentrated fraction under reduced pressure and dried in vacuum to obtain brownish red powder, which was analyzed as crocin by mass spectrometry, nuclear magnetic resonance and infrared -1, content is 98.7%.

Embodiment 2

[0018] Take ethyl acetate, ethanol, and water, mix them in a ratio of 5:3:4, let them stand in a separatory funnel for 8 hours, and separate the upper and lower phases. Take the upper phase and fill the high-speed countercurrent chromatographic column, turn the main engine at a speed of 1200rpm, pump the lower phase into the mobile phase, and when the mobile phase flows out, adjust the flow rate to 2ml / min, and take the mobile phase to dissolve gardenia yellow with a color value of 400 Pigment 1g, injected by the injection valve, detected by SP-200 ultraviolet detector, collected the target components according to the spectrum, concentrated fractions under reduced pressure and dried in vacuum to obtain brownish red powder crocin-I, the HPLC detection content was 98.1%.

Embodiment 3

[0020] Take ethyl acetate, ethanol, and water, mix them in a ratio of 6:4:5, let them stand in a separatory funnel for 12 hours, and separate the upper and lower phases. Take the upper phase and fill the high-speed countercurrent chromatographic column, turn the main engine at a speed of 800rpm, pump the lower phase into the mobile phase, and when the mobile phase flows out, adjust the flow rate to 1ml / min, and take the mobile phase to dissolve gardenia yellow with a color value of 400 Pigment 1g is sampled by the injection valve, detected by the SP-200 ultraviolet detector, and the target components are collected according to the spectrum, and the concentrated fraction is vacuum-dried to obtain brownish red powder crocin-I, and the HPLC detection content is 98.8%.

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Abstract

The invention belongs to the field of separation of natural products, in particular to a method for preparing crocin-I by high-speed countercurrent chromatography. The method is to take ethyl acetate, ethanol and water to mix and separate layers, take the upper phase to fill the high-speed countercurrent chromatographic column, turn the host, pump the lower phase into the mobile phase, dissolve the gardenia yellow pigment in the lower phase and inject the sample through the injection valve , detected by an SP-200 ultraviolet detector, collect the target components according to the spectrum, and dry the fraction under reduced pressure to obtain. The process of the invention is simple in operation, short in preparation period and high in yield, can obtain more than 98% of the crocin-I product, and can realize continuous production.

Description

Technical field: [0001] The invention belongs to the field of separation of natural products, in particular to a method for preparing crocin-I by high-speed countercurrent chromatography. Background technique: [0002] Crocin I (Crocin I), molecular formula C 44 h 64 o 24 , with a molecular weight of 976.96, is a dibasic ester formed by combining carotenoid crocetin and two molecules of gentiobiose. The molecular structure is: [0003] [0004] Crocin-I is brown-red crystal, easily soluble in hot water, orange in color, slightly soluble in absolute ethanol, ether and other organic solvents. Among the natural pigments in the yellow system, crocin-I is relatively stable and has the characteristics of light resistance, heat resistance, metal ion resistance and chemical resistance, and the color tone change is basically not affected by pH, especially for protein and starch. It also has excellent dyeability and high safety. In addition, crocin-I also has anti-oxidation, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H13/06C07H1/08
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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