Propolis supercritical CO2 extract GC-MS fingerprint and construction method thereof

A GC-MS, fingerprint technology, applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as difficult extraction, and achieve the effects of easy mastery, good reproducibility and high precision

Inactive Publication Date: 2011-05-04
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Propolis Supercritical CO 2 The main components of the extract are highly volatile terpenes and esters. Some people have discussed propolis supercritical CO 2 The establishment of gas chromatography (GC) fingerprints of extracts (Ma Haile et al., Propolis supercritical CO 2 GC fingerprint study of the extract, Beekeeping Science and Technology 2005. (1), 36-38), but due to the GC analysis, the sample was extracted by dissolving in chloroform, centrifuging and filtering the supernatant with a microporous membrane , this sample processing method is effective for propolis supercritical CO 2 The most active terpenes in the extract are difficult to extract, leading to the use of GC fingerprints to identify propolis supercritical CO 2 The authenticity of the extract has certain limitations

Method used

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  • Propolis supercritical CO2 extract GC-MS fingerprint and construction method thereof
  • Propolis supercritical CO2 extract GC-MS fingerprint and construction method thereof
  • Propolis supercritical CO2 extract GC-MS fingerprint and construction method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1 Propolis supercritical CO 2 Establishment method of GC-MS standard fingerprint of extract

[0042] 1. Preparation of test samples

[0043] The propolis samples were frozen overnight in a refrigerator at -20°C, and the frozen propolis samples were crushed through a 20-mesh sieve with a high-speed pulverizer, and 200 g of the crushed propolis samples were weighed and placed in supercritical CO 2 The supercritical CO of propolis obtained after extraction in the extraction kettle for 4 h 2 Extract (3 parallel extractions per sample, mix the extracts well).

[0044] Propolis Supercritical CO 2 Extraction conditions: Extraction tank temperature 35 °C, pressure 25 MPa, separation tank temperature 40 °C, pressure 6~8 MPa, CO 2 Flow 20~30 L·h -1 .

[0045] , solid-phase microextraction method

[0046] Propolis Supercritical CO 2 The extract was crushed with an inkstone bowl, weighed 1.000g sample, placed in a 15mL sample bottle, sealed, and equilibra...

Embodiment 2

[0052] Example 2 Detection of 11 batches of propolis supercritical CO 2 Fingerprint of the extract

[0053] Take propolis supercritical CO 2 11 batches of extracts are detected by the method of Example 1, and the GC-MS collection of 11 batches of samples is obtained, as Figure 1 to Figure 11 shown. Through the comparison of 11 batches of GC-MS spectra, the common peaks were extracted and the characteristic common peaks were determined.

[0054] Established propolis supercritical CO 2 There are 8 characteristic common peaks in the GC-MS fingerprint of the extract. Now, the compound composition analysis, retention time, peak area and relative peak area of ​​1 batch of Heilongjiang No. 2 sample spectrum are listed as follows:

[0055] Peak No. 1, benzoylethylene diacetic acid, retention time RT is 9.60min, relative peak area is 16.84%;

[0056] Peak No. 2, benzyl alcohol, retention time RT is 13.64min, relative peak area is 58.59%;

[0057] Peak No. 3, 1-undecyne, ha...

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Abstract

The invention relates to the field of detection methods of active ingredients of functional foods, and discloses a propolis supercritical CO2 extract gas chromatography-mass spectrometer (GC-MS) fingerprint and a construction method thereof. The propolis supercritical CO2 extract GC-MS fingerprint has 8 common peaks, wherein the total length of the fingerprint is 60 minutes. The construction method comprises the following steps of: placing a propolis sample in a supercritical CO2 extraction kettle to extract so as to obtain a supercritical CO2 extract of the propolis; weighing the propolis sample and placing in a sample bottle to perform solid-phase micro-extraction; performing GC-MS analysis; and finally comparing the GC-MS fingerprints of propolis supercritical CO2 extracts in different regions, and extracting the common peaks to form the GC-MS fingerprint of the propolis supercritical CO2 extract. The invention has the advantages that: the fingerprint is convenient and stable, has high precision and repeatability, is easy to master and the like. The time for detecting the sample is short; and the obtained propolis supercritical CO2 extract contains more than 120 volatile components.

Description

technical field [0001] The invention relates to the field of detection methods for active ingredients in health food, in particular to the construction of propolis supercritical CO by solid phase microextraction and GC-MS combined technology 2 Extract fingerprint information and construction method. Background technique [0002] Propolis is rich in active substances such as flavonoids and terpenes, and has unique health care functions and medical value. Generally, a group of 50,000 to 60,000 bees can only produce 100 to 150 grams of propolis a year, and the annual output of propolis in my country is only about 300 tons, so propolis is a scarce resource. Numerous studies have shown that supercritical CO 2 Extraction technology is an important means to obtain highly active components in propolis, which has been applied in actual production. Supercritical CO of propolis compared with conventional ethanol extract 2 The types of extract components are more abundant, especiall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/08
Inventor 马海乐王蓓任晓锋曲文娟骆琳
Owner JIANGSU UNIV
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