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Method for detecting quercetin patuletin in marigold slag

A technology of quercetin and marigold dregs, which is applied in the field of detection of flavonoids, can solve the problems of environmental pollution, waste of resources, and unreported detection methods of quercetin, and achieve accurate and applicable detection. Strong performance and short detection time

Active Publication Date: 2019-01-15
CHENGUANG BIOTECH GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, marigolds are mainly used to produce lutein in the industry, and the by-product is marigold dregs. Every year, a large amount of flavonoids such as quercetin marigold are discarded together with marigold dregs, which not only wastes resources, but also pollutes the environment.
The preparation, separation and purification of quercetin tagetin have been reported in the literature, and the patent applications of application numbers CN201410708334.4 and CN201110075820.3 respectively report the extraction, separation and purification of quercetin tagetin from marigold and marigold residue. The method of the paper "Isolation and Structural Identification of Tagetin and Quercetin Tagetin" (Journal of Guangzhou Medical College, Vol. ; But there is no literature report on quercetin tagetin detection method

Method used

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  • Method for detecting quercetin patuletin in marigold slag
  • Method for detecting quercetin patuletin in marigold slag
  • Method for detecting quercetin patuletin in marigold slag

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: The specific steps of the detection method of quercetin tagetin in the present marigold dregs are as follows.

[0030] (1) Standard curve: Accurately weigh 10 mg quercetin tagetin standard (accurate to 0.1 mg) and place it in a 10 ml volumetric flask, dissolve it with chromatographic methanol and make it to volume to prepare a standard stock solution. Dilute the standard stock solution 2 times gradient step by step, make six gradient levels, measure the peak area value according to the above conditions, and use the peak area-concentration as the standard curve, see the standard curve figure 2 .

[0031] (2) Sample extraction: Accurately weigh 0.05g (accurate to 0.0001g) marigold slag sample in a 10ml volumetric flask, dilute to volume with methanol, and extract ultrasonically for 10min at 50°C and 1000HZ.

[0032] (3) Centrifugation: transfer the extract obtained in step (2) to a centrifuge tube, centrifuge at 0°C at a speed of 10,000 r / min for 1 min, and c...

Embodiment 2

[0046] Example 2: The specific steps of the detection method of quercetin tagetin in the present marigold dregs are as follows.

[0047] (1) Standard curve: same as Example 1.

[0048] (2) Sample extraction: Accurately weigh 0.20g (accurate to 0.0001g) marigold slag sample in a 25ml volumetric flask, dilute to volume with methanol, and extract ultrasonically for 15min at 40°C and 1000HZ.

[0049] (3) Centrifugation treatment: Transfer the extract obtained in step (2) to a centrifuge tube, centrifuge at 0°C at a speed of 10,000 r / min for 2 minutes, and concentrate the supernatant to one-fifth of the original volume by a rotary evaporator.

[0050] (4) Degreasing solvent degreasing: add an equal volume of petroleum ether to the concentrated solution obtained in step (3), and defat twice;

[0051] (5) Anion exchange resin treatment: After loading D941 anion exchange resin column, use 3BV, 4wt% HCl aqueous solution to pass through the resin layer at a flow rate of 1BV / h. After th...

Embodiment 3

[0057] Example 3: The specific steps of the detection method of quercetin in the marigold residue are as follows.

[0058] (1) Standard curve: same as Example 1.

[0059] (2) Sample extraction: Accurately weigh 0.5g (accurate to 0.0001g) sample of marigold residue in a 50ml volumetric flask, dilute to volume with methanol, and extract ultrasonically at 70°C and 1000HZ for 20min.

[0060] (3) Centrifugal treatment: Transfer the extract obtained in step (2) to a centrifuge tube, centrifuge at 0°C at a speed of 10,000 r / min for 3 min, and concentrate the supernatant to one-fifth of the original volume by a rotary evaporator.

[0061] (4) Degreasing with degreasing solvent: add an equal volume of vegetable oil extraction solvent to the concentrated solution obtained in step (3), and degrease 3 times; then concentrate to dryness with a rotary evaporator, and ultrasonically dissolve the dry matter with 5ml of 70vol% ethanol aqueous solution.

[0062] (5) Anion exchange resin treatm...

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Abstract

The invention discloses a method for detecting quercetin patuletin in marigold slag. The method comprises the steps that (1) a marigold slag sample is extracted through methyl alcohol, centrifuging isconducted through a high-speed refrigeration centrifuge, and supernatant is concentrated to obtain concentrated liquor; (2) the concentrated liquor is degreased through a degreasing solvent and thendried by evaporation to obtain a dried material; (3) the dried material is dissolved with an ethanol aqueous solution, then sequentially purified by anion exchange resin and cationic exchange resin, and column passing liquid is collected; (4) the column passing liquid is dried by evaporation and subjected to volume metering through a methanol aqueous solution; and (5) a sample solution is detectedthrough an ultrahigh-efficiency liquid chromatogram-ultraviolet method, and quantified through an external standard method. According to the method, high-speed refrigeration centrifuging, degreasingthrough the degreasing solvent and purifying through the cationic exchange resin are conducted, thus interference of the vast majority of impurities is eliminated, metal ion interference is eliminated, and detection is accurate; and the ultrahigh-efficiency liquid chromatogram detecting metho quite high in applicability and short in detection time is established.

Description

technical field [0001] The invention relates to a detection method of flavonoid components, in particular to a detection method of quercetin tagetes in marigold dregs. Background technique [0002] Marigold is widely planted all over the world. In addition to its ornamental value, it also has good medicinal value. Its functional components mainly include carotenoids, flavonoids, terpenoids and essential oils. Among them, quercetin tagetin is a unique flavonoid compound of marigold flavonoids, which has antioxidant activity of scavenging free radicals and strong anti-tumor effects. [0003] At present, marigolds are mainly used to produce lutein in the industry, and the by-product is marigold dregs. Every year, a large amount of flavonoids such as quercetin marigold are discarded together with marigold dregs, which not only wastes resources, but also pollutes the environment. . The preparation, separation and purification of quercetin tagetin have been reported in the liter...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/74
CPCG01N30/02G01N30/06G01N30/74G01N2030/027G01N2030/062
Inventor 张晓芳吉桂珍张玉芬刘登帅栗星
Owner CHENGUANG BIOTECH GRP CO LTD
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