Method for preparing high-content trans-lutein crystals from dried marigold flower pellets

A trans-lutein, high-content technology, applied in the direction of organic chemistry, can solve problems such as lutein decomposition, achieve accurate qualitative and quantitative analysis, shorten the reaction time, and reduce the residual amount of organic solvents.

Inactive Publication Date: 2010-07-14
JIANGSU ACADEMY OF AGRICULTURAL SCIENCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Studies have shown that tetrahydrofuran is prone to form

Method used

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  • Method for preparing high-content trans-lutein crystals from dried marigold flower pellets
  • Method for preparing high-content trans-lutein crystals from dried marigold flower pellets
  • Method for preparing high-content trans-lutein crystals from dried marigold flower pellets

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030]Grind the dried marigold flower particles through a 20-mesh sieve, weigh 1 kg of marigold pollen, add 3 liters of petroleum ether (boiling range 30-60°C), 2 liters of 100 g / L potassium hydroxide ethanol solution, and reflux at 55°C for extraction Saponification for 3 hours. Extract the saponification liquid and filter to remove the filter residue, concentrate the filtrate under reduced pressure at 35-45°C until there is no distillate, then add 0.6 liter of 50% ethanol aqueous solution to the concentrated solution, stir well, and add 25% acetic acid aqueous solution to adjust the pH value to 7.0, after the crystallization of trans-lutein, centrifuge at 5000 rpm for 15 minutes, pour off the supernatant to obtain a precipitate containing trans-lutein, and vacuum freeze-dry to obtain the crude product of trans-lutein 230.4 gram, the vacuum degree during vacuum freeze-drying is 15-50Pa, the temperature is lower than -40°C, and the drying time is 20-24 hours. As detected by H...

Embodiment 2

[0033] Grind the dried marigold flower particles through a 40-mesh sieve, weigh 0.8 kg of marigold pollen, add 3.2 liters of petroleum ether (boiling range 30-60°C), 2.5 liters of 100 g / L potassium hydroxide ethanol solution, and reflux at 60°C for extraction Saponified for 2.5 hours. Extract the saponification liquid and filter to remove the filter residue, concentrate the filtrate under vacuum at 35-45°C until there is no distillate, then add 0.5 liter of 50% ethanol aqueous solution to the concentrated solution, stir well, and add 25% acetic acid aqueous solution to adjust the pH value to 7.0, after the crystallization of trans-lutein, centrifuge at 5000 rpm for 15 minutes, pour off the supernatant, obtain a precipitate containing trans-lutein, and vacuum freeze-dry to obtain the crude product of trans-lutein 237.4 grams, detected by HPLC, the yield of trans-lutein was 1.450%. The crude trans-lutein was dissolved in 1.5 liters of ethyl acetate, washed with 1.5 liters of de...

Embodiment 3

[0035] Grind the dried marigold flower granules through a 40-mesh sieve, weigh 0.9 kg of marigold pollen, add 2.7 liters of petroleum ether (boiling range 30-60°C), 1.5 liters of 100 g / l potassium hydroxide ethanol solution, and reflux at 58°C for extraction Saponification for 3 hours. Extract the saponification liquid and filter to remove the filter residue, concentrate the filtrate under vacuum at 35-45°C until there is no distillate, then add 0.7 liters of 50% ethanol aqueous solution to the concentrated solution, stir well, and add 25% acetic acid aqueous solution to adjust the pH value to 7.0, after the crystallization of trans-lutein, centrifuge at 5000 rpm for 15 minutes, pour off the supernatant to obtain a precipitate containing trans-lutein, and vacuum freeze-dry to obtain the crude product of trans-lutein 240.5 grams, detected by HPLC, the yield of trans-lutein was 1.487%. The crude trans-lutein was dissolved in 1.5 liters of ethyl acetate, washed with 1.5 liters o...

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Abstract

The invention relates to a method for preparing high-content trans-lutein crystals from dried marigold flower pellets. The method includes the following steps that: after the dried marigold flower pellets are ground and sieved, organic solvent and aqueous alkali are added to carry out extraction and saponification at the same time, the extracted saponified solution is filtered to remove filter residue, and is then concentrated under vacuum, 50 percent of aqueous ethanol solution is then added into the concentrated solution, the pH value is regulated to 7.0, and after centrifugation and vacuum freeze drying, crude trans-lutein is obtained. The crude trans-lutein is dissolved in ethyl acetate, and is washed by deionized water, the ethyl acetate phase is concentrated under vacuum, normal hexane/acetone mixed solvent is added in the concentrated solution, the concentrated solution is kept still under the room temperature and then filtered, and is then washed by cold ethanol and deionized water, and after vacuum freeze drying, the high-content trans-lutein crystal is prepared. The invention has the advantages of simple technique and high trans-lutein yield, and is suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for preparing high-content trans-lutein crystals from dry marigold flower granules. Background technique [0002] Marigold is a natural raw material rich in lutein substances, and marigold extract has been commercialized internationally. Lutein belongs to the carotenoid tetraterpenoids, which are widely found in flowers, fruits, vegetables and other plants. Lutein with higher purity is an orange-yellow powder with a weak hay smell. It is insoluble in water, methanol and other polar solvents, and easily soluble in tetrahydrofuran, ethyl acetate, petroleum ether and other organic solvents with low polarity. in solvent. The potential value of lutein includes improving immune function, inhibiting cytoplasmic self-oxidation, protecting cell units from damage caused by oxidants, treating cancer, and preventing macular degeneration in the elderly. At present, the preparation process of lutein substances, such as chemical s...

Claims

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Application Information

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IPC IPC(8): C07C403/24
Inventor 李大婧王闯宋江峰刘春泉
Owner JIANGSU ACADEMY OF AGRICULTURAL SCIENCES
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