Method for analyzing propolis chemical components through pyrolysis gas chromatography-mass spectrometry

A technology for cracking gas chromatography and chemical components, applied in the field of analysis of chemical components of propolis, can solve the problems of complicated operation, laborious, difficult to react to the composition and characteristics of propolis, simplifies experimental steps, saves experimental time, and has far-reaching rapid evaluation. Effect

Active Publication Date: 2013-09-25
上海鹿明生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This requires the samples to be processed separately, the operation is complex, time-consuming and laborious, and it is difficult to reflect the composition and characteristics of the overall chemical composition of propolis
At present, there is no relevant report on propolis cracking gas chromatography mass spectrometry analysis, so the present invention has established a kind of cracking chromatography mass spectrometry analysis method that can fully reflect the partial chemical composition such as volatile oil, resin, beeswax in propolis, can simultaneously to a certain extent The method to reflect the quality of propolis has important academic research value and practical application value

Method used

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  • Method for analyzing propolis chemical components through pyrolysis gas chromatography-mass spectrometry
  • Method for analyzing propolis chemical components through pyrolysis gas chromatography-mass spectrometry
  • Method for analyzing propolis chemical components through pyrolysis gas chromatography-mass spectrometry

Examples

Experimental program
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Effect test

Embodiment 1

[0024] The selection of embodiment 1 cracking temperature

[0025] (1) Instruments and reagents

[0026] American Thermo Finnigan Trace DSQ gas chromatography / mass spectrometry (GC-MS); American Varian CP-3800 gas chromatograph with hydrogen flame detector (FID); Japanese Frontier PY-2020iD double-click vertical micro furnace cracker .

[0027] Purchase fresh propolis glue from Shandong Tai'an, Shandong Linyi, Hubei, and Zhejiang bee farms, remove visible sawdust, bee corpses and other debris, freeze overnight at -20°C, take it out and quickly grind it through a 120-mesh sieve to make propolis powder. spare.

[0028] (2) Experimental method

[0029] 1) Selection of pyrolysis temperature

[0030] Accurately weigh 0.1 mg of Shandong Taian propolis powder and put it into the sample cup, fix it on the injection rod, and put it into the cracker installed above the GC inlet, and the sample is at room temperature at this time. After the temperature of the cracker reaches the app...

Embodiment 2

[0036] The investigation of embodiment 2 reproducibility

[0037] American Varian3800 gas chromatograph (UA-5 metal capillary column, 30m×0.25mm i.d.×0.25μm, film thickness 5% methylpolysiloxane, Japan), Japan Frontier PY-2020iD double-click vertical micro-furnace cracker.

[0038] Gas phase conditions: heating program: initial temperature 40°C, rise to 300°C at a rate of 10°C / min, and keep for 10 minutes; inlet temperature is 300°C, detector temperature is 300°C, split ratio 30:1; carrier gas nitrogen or Helium, flow rate 1.0mL / min.

[0039] Cracker conditions: cracking furnace temperature: 550°C; interface temperature between cracker and gas chromatograph: 350°C;

[0040] Accurately weigh 3 parts of Shandong Tai'an propolis powder 0.1 mg prepared by the method in Example 1, put them into a sample cup, fix it on the sample rod, and put it into the cracker installed above the GC sample inlet, and the sample is at room temperature at this time. When the temperature of the cra...

Embodiment 3

[0042] Embodiment 3 propolis content analysis

[0043] Gas chromatography / mass spectrometry (GC-MS) from Thermo Finnigan Trace DSQ in the United States; Frontier PY-2020iD double-click vertical micro-furnace cracker from Japan.

[0044] The gas phase conditions are: the chromatographic column is a UA-5 metal capillary column (30m×0.25mm i.d.×0.25μm, film thickness 5% methyl polysiloxane, Japan). The min rate was increased to 300°C and kept for 5min; the inlet temperature was 300°C, the detector temperature was 300°C, the split ratio was 30:1; the carrier gas was nitrogen or helium, and the flow rate was 1.0mL / min.

[0045] The mass spectrometry conditions are: electron bombardment ion source, ion source temperature 230°C, transfer line temperature 300°C, ionization energy 70eV, ion scanning range 40-550m / z.

[0046] Cracker conditions: cracking furnace temperature: 550°C; interface temperature between cracker and gas chromatograph: 350°C.

[0047] Accurately weigh 0.1 mg of ...

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Abstract

The invention discloses a method for analyzing propolis chemical components through pyrolysis gas chromatography-mass spectrometry. The method comprises the steps that: propolis powder is placed in a pyrolysis device; the pyrolysis device is placed at a feeding port of a gas chromatograph; when the temperature of the pyrolysis device reaches 400-600 DEG C, feeding is carried out; with a method in which a linear temperature increasing retention index is combined with a mass spectrometry standard spectral library, the chemical components of the propolis are qualified; and the propolis chemical components are subjected to quantitative analysis through calculating areas of the peaks in the gas chromatography spectrum. Solid sample is directly fed into pyrolysis gas chromatography, and no solvent is adopted, such that operation is simple and environment-friendly. The pyrolysis gas chromatography-mass spectrometry method is developed for carrying out qualitative and quantitative detections upon the pyrolysis sample, such that experiment time can be effectively saved, experiment steps can be simplified, and propolis quality can be rapidly evaluated. The detection technology can be popularized to a pyrolysis quality detection field, and has an important significance upon rapid evaluation of pyrolysis quality.

Description

(1) Technical field [0001] The invention relates to a method for analyzing chemical components of propolis, in particular to a method for analyzing chemical components of propolis by pyrolysis gas chromatography-mass spectrometry. (2) Background technology [0002] Propolis is a resin that bees collect from tree buds, bark and other parts of plants, mixed with glandular secretions such as bee tongue glands and wax glands, and processed and transformed by bees into a gelatinous substance. The composition of propolis is extremely complex, and its basic components are: 50% to 55% resins, 10% volatile oil, 30% to 40% beeswax, and 5% pollen. In terms of chemical composition, there are mainly flavonoids, organic acids, aldehydes, alcohols, alkenes, hydrocarbons, terpenoids, etc. It is generally believed that the biological activity of propolis mainly comes from flavonoids, phenolic acids and volatile oils in the resin. terpenes and their derivatives etc. [0003] Different compo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 王丽丽杨红丽黄翌磊董文霞潘再法
Owner 上海鹿明生物科技有限公司
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