Method for determining sterol content by utilizing quantitative nuclear magnetic resonance technology

A technology of nuclear magnetic resonance and proton nuclear magnetic resonance spectrum, which is applied in the direction of using nuclear magnetic resonance spectrum for measurement, using nuclear magnetic resonance for analysis, magnetic resonance measurement, etc., can solve the problems of inaccurate measurement results, interference, and inaccurate results.

Active Publication Date: 2016-12-07
OCEAN UNIV OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can only determine the content of several known sterols, ignoring other unknown components with similar structures, so that the result of the total content is not accurate enough
There are also reports on the determination of sterol content by nuclear magnetic resonance technology, but the selected quantitative peak is easily interfered by other peaks, and the measurement results are also not accurate enough

Method used

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  • Method for determining sterol content by utilizing quantitative nuclear magnetic resonance technology
  • Method for determining sterol content by utilizing quantitative nuclear magnetic resonance technology
  • Method for determining sterol content by utilizing quantitative nuclear magnetic resonance technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: the mensuration of phytosterol total content in seaweed

[0020] (1) Preparation of test solution

[0021] Accurately weigh 750mg of hijiki coarse powder, add 4.8mL of distilled water, soak at room temperature for 15min; add 12mL of methanol, 6mL of dichloromethane (containing 0.01% BHT), shake for 2min; add 6mL of dichloromethane for shaking for 30s; add 6mL of water for shaking for 30s Centrifuge at 5000rpm for 15min, discard the supernatant; add 15g of anhydrous sodium sulfate, shake for 1h, filter, and concentrate to obtain total fat. Add 1mL of 1M KOH / 80% ethanol to the total lipid, saponify at room temperature for 15h in the dark; add 2mL of water to the reaction liquid, extract with 3mL ether, twice in total; combine ether layer, wash with 4mL water until neutral, N 2 Blow dry to obtain ether extract.

[0022] With 2,3,4,5-tetrachloronitrobenzene as the internal standard and deuterated chloroform as the solvent, an internal standard solution with ...

Embodiment 2

[0047] Embodiment 2: Determination of the total content of phytosterols in Hijiki extract

[0048] Accurately weigh 2 g of different batches of hijiki extracts, add 1.5M potassium hydroxide ethanol solution according to the ratio of solid to liquid at 1:10, and react at 70°C for 1.5 h to obtain a reaction solution. Cool to room temperature, add 1 times the amount of diethyl ether for extraction, and extract twice in total, combine the diethyl ether layers, wash with water until neutral, and blow dry with nitrogen to obtain the diethyl ether extract. With 2,3,4,5-tetrachloronitrobenzene as the internal standard and deuterated chloroform as the solvent, prepare an internal standard solution with a concentration of 1.0 mg / mL. Accurately pipette 0.4mL internal standard solution to dissolve the above-mentioned dried ether extract, and after fully dissolving, the test solution is obtained.

[0049] Carry out proton nuclear magnetic resonance spectrum determination according to embo...

Embodiment 3

[0052] Embodiment 3: the mensuration of phytosterol total content in corn oil

[0053] Accurately take by weighing each 200mg of different batches of corn oil, and prepare the test solution with Example 2.

[0054] Carry out proton nuclear magnetic resonance spectrum measurement by embodiment 1 step (2), carry out integral processing to proton spectrum, according to the formula (1) in embodiment 1, M f The total content of phytosterols in corn oil was obtained based on the molecular weight of β-sitosterol, a representative component in the test sample, which was 414.7. The specific results are shown in Table 3.

[0055] Table 3 Total content of phytosterols in different batches of corn oil

[0056]

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Abstract

The invention relates to a method for determining content of sterol and/or derivatives thereof by utilizing a quantitative nuclear magnetic resonance technology. The method comprises the following steps: adopting a nuclear magnetic resonance internal standard method, selecting a specific quantitative peak of sterol and/or derivatives thereof, and accurately determining (total) content of the sterol and/or derivatives thereof. The method provided by the invention has the advantage that extracts of animals, plants and/or microorganisms, food, medicines or the content of sterol and/or derivatives thereof in cosmetics can be accurately determined.

Description

technical field [0001] The invention provides a method for determining the content of sterols and / or derivatives thereof by using hydrogen nuclear magnetic resonance spectroscopy. Background technique [0002] Sterols and their derivatives include natural and synthetic sterols and their derivatives. Natural sterols and their derivatives include plant and animal sterols and their derivatives. Among them, phytosterols (plant sterols) are a class of natural alcohol compounds with cyclopentane perhydrophenanthrene (steroid nucleus) as the skeleton, and are one of the components of cell membranes in plants. The structure of this type of compound is similar to that of cholesterol, and has the functions of lowering cholesterol and preventing and treating cardiovascular diseases. It is a kind of safe and effective natural phytochemicals. In 1999, the U.S. Food and Drug Administration (FDA) has approved the use of "healthy" labels for foods added with phytosterols. In 2000, the U....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08G01N1/28
CPCG01N1/28G01N24/082G01N24/08G01N2001/2893G01R33/46G01N1/38
Inventor 刘红兵王聪张秀丽张培育
Owner OCEAN UNIV OF CHINA
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