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A kind of naringenin standard substance and its preparation and application

A naringenin, preparation-type technology, applied in the field of naringenin preparation, can solve the problems of high manufacturing cost, undisclosed naringenin standard substance preparation method, complexity, etc., and achieve large mass transfer coefficient and adjustable solubility , highly selective effect

Inactive Publication Date: 2016-04-20
NAT INST OF METROLOGY CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the preparation of standard substances is often much more complicated than conventional analytical chemical reagents, often requires a variety of high-precision separation and purification steps (such as HPLC, etc.), and also causes its high manufacturing cost
[0008] Although there are naringenin standard substances available in the prior art, the preparation methods of these naringenin standard substances are not disclosed

Method used

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  • A kind of naringenin standard substance and its preparation and application
  • A kind of naringenin standard substance and its preparation and application
  • A kind of naringenin standard substance and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0098] Embodiment 1. The preparation of naringenin

[0099] The method for preparing purified naringenin from citrus peel, its concrete steps are as follows:

[0100] (1) Turn on the cooling heat exchanger to lower the temperature to about -5°C;

[0101] (2) Pack the pretreated experimental raw materials into the extraction kettle and seal it;

[0102] (3) Check and ensure that the back pressure valve is closed and the inlet valve of the high pressure pump is opened;

[0103] (4) Turn on the main power of the incubator 30 minutes before the operation and set the temperature of the extraction kettle and the separation kettle;

[0104] (5) Open the cylinder valve after the temperature meets the requirements;

[0105] (6) Turn on the high-pressure pump, observe the pressure on the computer screen, and confirm that the pressure meets the requirements;

[0106] (7) Before the pressure reaches the expected value, especially when it reaches about 10MPa, especially observe the val...

Embodiment 2-6

[0125] Except for the technical parameters listed in the table below, other preparation methods are the same as in Example 1 (see table 1 below for details).

[0126] Table 1

[0127]

[0128] Similarly, the pure product of naringenin prepared in Example 2-6 was identified by HPLC-MS (ScanESI-MS) and HPLC fixed-value spectrum, which all showed that the naringenin was obtained by the extraction and separation method of Example 2-6. white.

Embodiment 7

[0129] The selection of the HPLC analysis condition of embodiment 7.naringenin standard substance

[0130] 7.1 Preparation of the test solution

[0131] Accurately weigh 10 mg of pure naringenin prepared in Example 1 and place it in a 5 mL volumetric flask, add an appropriate amount of water to dissolve and dilute to the mark to obtain a naringenin solution with a concentration of 2 mg / mL, which is used to determine the chromatographic separation conditions and fixed value use.

[0132] 7.2 Determination of chromatographic conditions

[0133] 7.2.1 Selection of mobile phase

[0134] The mobile phase composed of different ratios of water:methanol was investigated respectively, and 15%:85% (water:methanol) was selected as the mobile phase.

[0135] 7.2.2 Selection of chromatographic column:

[0136] The C18 chromatographic column was selected for testing, and the final chromatographic conditions were as follows:

[0137] Chromatographic column: Agilent ZORBAXExtend-C1821.2*...

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Abstract

The invention provides a method for extracting and separating high-purity naringenin from citrus peel. According to the method, the high-purity naringenin product with the purity reaching up to 99.5% can be prepared by a supercritical fluid extraction technique and a preparative high performance liquid chromatography, and the preparation requirements of a standard substance can be met.

Description

technical field [0001] The invention relates to a method for preparing naringenin, in particular to a method for preparing high-purity naringenin from citrus peels by using supercritical fluid extraction technology and preparative high-performance liquid chromatography, and the pomelo obtained by the preparation method Use of corticosteroids as standard substances. Background technique [0002] Naringenin is a polyhydroxy flavonoid monomer component in Rutaceae citrus plants, and is an aglycone of naringin. Naringenin is a white crystalline fine powder, belonging to dihydroflavonoids, white needle-like crystals, melting point 260°C, naringenin is soluble in methanol, ethanol, ether and benzene, almost insoluble in water, the molecule shows medium polarity, molecular formula for C 15 h 12 o 5 , the molecular weight is 272.25, and its structural formula is as follows: [0003] [0004] Since naringenin contains functional groups such as benzene ring, hydroxyl group and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/32C07D311/40G01N33/00
CPCC07D311/32C07D311/40G01N30/88Y02P20/54
Inventor 全灿马康韩强
Owner NAT INST OF METROLOGY CHINA
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