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Detection method of corn oil unsaponifiable matter fingerprint spectrum and standard fingerprint spectrum of corn oil unsaponifiable matter fingerprint spectrum

A standard fingerprint and fingerprint technology, which is applied in the detection field of corn oil unsaponifiable matter fingerprint, can solve the problems of few, unsuitable, and incomplete separation components, achieve good reproducibility, good separation effect, and prevent adulteration fake effect

Pending Publication Date: 2022-04-15
湖南天龙制药有限公司
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

Rice bran oil is mainly fatty acid, which is completely different from the composition of this product. This product is the unsaponifiable product obtained by saponifying corn oil. Therefore, the fingerprint method established by it can only be used for the identification of rice bran oil, not for unsaponifiable object identification
[0024] 2. Su Qingyun and others separated the unsaponifiable components of selenium-enriched corn oil, and only identified four sterol acetates, while the unsaponifiables of corn oil are multi-component compounds. In addition to sterols, there are vitamin E, Dozens of components such as squalene and higher alcohols, so this method is not comprehensive, and it is not suitable for the identification of all components of corn oil unsaponifiable matter
[0025] 3. In the patent of Wang Qiang_Zhang Jianshu and others, the separation of components by HPLC method is relatively small and incomplete. The four isomers of vitamin E (tocopherol) were not detected, and other sterols and higher alcohols were not detected.
[0026] 4. Shen Ping and others used preparative high performance liquid chromatography to separate the unsaponifiable matter of rapeseed oil into four types: sterols, 4-methyl sterols, triterpene alcohols and hydrocarbons. Separation and structural analysis of sterols and other components, but no research on vitamin E, squalene, cetyl alcohol, stearyl alcohol, etc., and no research on other oils
[0027] Above, there is no GC method for chromatographic separation of vegetable oil unsaponifiables, establishment of standard fingerprints, and component identification of each chromatographic peak in the chromatogram

Method used

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  • Detection method of corn oil unsaponifiable matter fingerprint spectrum and standard fingerprint spectrum of corn oil unsaponifiable matter fingerprint spectrum
  • Detection method of corn oil unsaponifiable matter fingerprint spectrum and standard fingerprint spectrum of corn oil unsaponifiable matter fingerprint spectrum
  • Detection method of corn oil unsaponifiable matter fingerprint spectrum and standard fingerprint spectrum of corn oil unsaponifiable matter fingerprint spectrum

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0095] Optimization of Fingerprint Detection Method

[0096] 1. The optimization of the test solution treatment method

[0097] The preparation method of the test solution is as follows: Weigh 100-200mg of corn oil unsaponifiable matter sample, put it in a 10mL measuring bottle, add an organic solvent into the measuring bottle, ultrasonicate for 5 minutes to dissolve the sample, and filter through a microporous membrane. , make to volume, shake well, set aside. We focus on optimizing the solvent. According to the fat-soluble physical properties of the unsaponifiable matter of corn oil, the commonly used organic solvents methanol, ethanol, ethyl acetate, chloroform, petroleum ether, and n-hexane were used for testing. The results are shown in Table 1 below:

[0098] Table 1 Solvent optimization experiment results

[0099] Choose a solvent Test article solubility Interference with chromatograms Status of chromatographic peaks methanol insoluble only so...

Embodiment 2

[0119] The establishment process of standard fingerprint

[0120] 1. Confirmation of each chromatographic peak in the fingerprint

[0121] If the test product contains the same components as the standard product, there will be a chromatographic peak with the same retention time as the standard product in its chromatogram, and then it can be preliminarily identified what kind of substance each chromatographic peak belongs to.

[0122] 1.1 Standard solution preparation:

[0123] As mentioned above in the technical background, about the composition of corn oil unsaponifiable matter, there are still 4 problems that have not been clarified in the existing research and literature reports. Since it is not possible to determine how many characteristic components there are, according to the existing literature reports and the inventor's analysis conjecture, select the functional components and characteristic components that may exist in the test product as standard products, and accur...

Embodiment 3

[0151] Analytical Method Validation

[0152] In order to ensure the reliability of the fingerprint detection method, the specificity, repeatability, intermediate precision and other items were verified. The results are as follows.

[0153] 3.1. Specificity

[0154] Precisely draw 1 μL each of n-hexane, β-sitosterol, and sample solution, inject them into the GC instrument respectively, and analyze according to the above-mentioned chromatographic conditions. The results are shown in Figures 11 to 13 , the experiment shows that: the solvent has no interference, and there is a chromatographic peak of β-sitosterol in the sample.

[0155] 3.2 Repeatability

[0156] Weigh corn unsaponifiable matter ①0.1004g ②0.1021g ③0.1032 ④0.1028 ⑤0.1047g ⑥0.1207g respectively from a batch of standard samples and put them in a 10ml volumetric flask and add n-hexane to dilute to the mark. Peak time and peak area. Based on the fact that β-sitosterol is a stable active ingredient, it is used to c...

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Abstract

The invention relates to the field of pharmaceutical analysis and quality control, and particularly discloses a corn oil unsaponifiable matter fingerprint detection method, a standard fingerprint and application thereof. The detection method comprises preparation of a test solution, preparation of a reference solution, chromatographic conditions and GC determination: after a chromatogram is obtained, an effective component chromatographic peak with good reproducibility and a large peak area ratio is selected from the chromatogram as a characteristic peak, and then a standard fingerprint spectrum is established. During application, two core parameters, namely the relative peak area ratio and the relative retention time, are selected, and the similarity between a sample chromatogram and a standard fingerprint spectrum is obtained according to a certain calculation method, so that the consistency between the sample and the standard fingerprint spectrum is determined. The detection method and the standard fingerprint spectrum can be finally used as an effective quality control means for identifying the authenticity and the quality of the unsaponifiable corn oil product, and adulteration can be prevented.

Description

technical field [0001] The invention relates to the fields of drug analysis and quality control, and in particular discloses a detection method for the fingerprint of unsaponifiable matter of corn oil, a standard fingerprint and an application thereof. Background technique [0002] Under certain chromatographic conditions, the extract of traditional Chinese medicine (or Chinese patent medicine) can obtain a chromatogram after chromatographic analysis. Although it is not yet possible to explain the attribution of each chromatographic peak on the picture, it can at least prove the existence of its corresponding components. Therefore, these chromatographic peaks constitute the intrinsic quality of the tested Chinese medicine. Since the internal component spectrum of each traditional Chinese medicine is relatively fixed, and the component spectrum of different traditional Chinese medicines is absolutely different, it has the same identification function as a human fingerprint wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N30/8686G01N2030/065
Inventor 龙建蒋孟良曾彦刘党生
Owner 湖南天龙制药有限公司
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