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Method for preparing and determining value of hesperetin reference material

A standard substance, orange peel technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of small quantity, the technical level of preparation and determination needs to be improved, and the type is single, and achieve stable sample properties and characteristic quantitative values. Accurate and reliable results with accurate and reliable results

Active Publication Date: 2018-11-30
SOUTHWEST UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although flavonoids have been widely used in the fields of food, medicine, and cosmetics, the number of such reference materials in my country is small and the types are single, and the technical level of preparation and valuation of related reference materials needs to be improved.

Method used

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  • Method for preparing and determining value of hesperetin reference material
  • Method for preparing and determining value of hesperetin reference material
  • Method for preparing and determining value of hesperetin reference material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1 standard substance sample preparation

[0028] 1. Preparation of standard materials

[0029] Candidate tangeretin, a reference material, was purchased from Nanjing Caobenyuan Biotechnology Co., Ltd., and was purified using reversed-phase C18 silica gel. Purification conditions: the amount of reversed-phase silica gel was 150 g, the loading amount was 400 mg, and the eluent ratio was water: acetone volume ratio for 30:70. After purification, rotary evaporation was performed, and the purity of the sample was detected by HPLC, such as figure 1 As shown, the purity of hesperetin after purification is increased from 98.29% to 99.98%, and the purification effect is remarkable. Subsequent drying is carried out in an oven and freeze-drying method, and the moisture content is reduced to 0.0251%. After dehydration and drying, mix well, place in a clean and dry packaging environment, dispense into 4mL clean Agilent brown glass bottles, tighten and cover well. Each...

Embodiment 2

[0045] Embodiment 2 standard substance fixed value

[0046] Referring to the "National Primary Standard Standard Material Technical Specification", through the previous literature research and pre-experimental results, this study adopts two different principles of liquid chromatography area normalization method and differential calorimetry scanning method to determine the purity standard material of orange peel Value. The liquid chromatography area normalization method includes HPLC-UV method to determine the main component of hesperetin, Karl Fischer Coulomb method to determine water content, headspace gas chromatography to determine volatile impurity content, and ICP-MS and ICP-OES to determine inorganic Element content, etc., in order to ensure the traceability and accuracy of the measurement results, the instruments and equipment used have undergone metrological verification or standard material calibration.

[0047] Valuation method 1: high performance liquid chromatogra...

Embodiment 3

[0129] Embodiment 3 Uncertainty evaluation

[0130] The source analysis and evaluation process of the uncertainty source of orange peel purity reference material is as follows: Figure 4 shown. The uncertainty of the purity standard substance of orange peel is composed of three parts: the uncertainty u introduced by the uniformity of the standard substance bb ; The uncertainty introduced by the stability of the standard substance (short-term stability u lts and long-term stability u sts ) and the uncertainty u introduced by the process of determining the value of the standard substance char .

[0131] 1. Uncertainty introduced by uniformity

[0132] According to the requirements of technical specifications, the homogeneity evaluation was carried out by one-way analysis of variance. Uniformity standard deviation s H It can be calculated with the formula:

[0133]

[0134] In the formula: sH is the standard deviation of uniformity; is the variance between groups; ...

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Abstract

The invention discloses a method for determining the value of a hesperetin reference material. The steps are as follows: 1) the mass percentage content of hesperetin in hesperetin raw material powderis determined by high performance liquid chromatography area normalization method, and the purity value P0 of the hesperetin raw material powder is obtained; 2) the mass percentage contents of water,organic volatile impurities and organic non-volatile impurities in the hesperetin raw material powder are determined, hesperetin purity value PHPLC-AN = P 0 * [100%-Xw-Xn-Xv] * 100% is determined by combination of the P0 determined by the step 1); 3) hesperetin purity value PDSC is determined by differential scanning calorimetry (DSC); and 4) final hesperetin purity value is calculated. The invention discloses a method for preparing the hesperidin reference material. The method for preparing the hesperidin reference material is as follows: first, preparing the reference material, to be more specific, taking a candidate reference material, purifying the candidate reference material with reverse C18 silica gel, performing rotary evaporateion, drying and storing; and determining the purity value according to the method for determining the value.

Description

technical field [0001] The invention relates to a method for determining a value of a standard substance, in particular to a method for preparing and determining a value of a standard substance of tangeretin. Background technique [0002] Flavonoids (Flavonoids) are an important class of secondary metabolites in plants, which exist in many food-derived plants such as fruits, vegetables, beans and tea in the form of bound (flavonoid glycosides) or free (flavonoid aglycones) . Flavonoids, especially polymethoxylated flavonoids, have significant physiological effects such as enhancing human immunity, anti-cancer, antibacterial and anti-inflammatory, preventing diabetes and cardiovascular and cerebrovascular diseases. Therefore, they are currently widely added as important ingredients in dietary supplements and other functions Sexual health food. At the same time, according to the different components and contents of flavonoids, it can also be used as a characteristic indicato...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027
Inventor 苏学素焦必宁李珍柱王敏周剑杨梦瑞王彤彤
Owner SOUTHWEST UNIVERSITY
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