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Method for identifying fritillaria thunbergii, fritillaria cirrhosa and fritillaria ussuriensis with pyrolysis-gas chromatography fingerprints

A technology of pyrolysis gas chromatography and gas chromatography, which is applied in the field of Chuan Fritillaria and Pyramid Fritillaria, combining cracking-gas chromatography with fingerprints to identify Zhejiang Fritillaria, can solve the problems of lack of conjugate bonds, poor volatility of alkaloids, and consume a lot of time and effort. Solve problems such as organic solvents, achieve the effect of saving experimental time, simplifying experimental steps, and easy operation

Inactive Publication Date: 2018-11-20
ZHEJIANG UNIV OF TECH
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  • Abstract
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AI Technical Summary

Problems solved by technology

At present, the analysis methods of alkaloids mainly include gas chromatography and liquid chromatography. Due to the poor volatility of alkaloids and the lack of conjugate bonds in the structure of most isosteroid alkaloids, it is necessary to add light-absorbing groups by derivatization methods , make it absorb ultraviolet light or silanize, improve its volatility and detection sensitivity, which requires complex sample pretreatment, consumes a lot of time and organic solvents, and it is difficult to fully reflect the composition and characteristics of the chemical components of Fritillaria
At present, there is no relevant report on the identification of Fritillaria fritillaria by gas chromatography combined with modes, so the present invention establishes a cracking chromatographic analysis method that can fully reflect the chemical composition of Fritillary fritillary, and combined with fingerprints to identify the types of Fritillaria , has important academic research value and practical application value

Method used

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  • Method for identifying fritillaria thunbergii, fritillaria cirrhosa and fritillaria ussuriensis with pyrolysis-gas chromatography fingerprints
  • Method for identifying fritillaria thunbergii, fritillaria cirrhosa and fritillaria ussuriensis with pyrolysis-gas chromatography fingerprints
  • Method for identifying fritillaria thunbergii, fritillaria cirrhosa and fritillaria ussuriensis with pyrolysis-gas chromatography fingerprints

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The selection of embodiment 1 cracking temperature

[0031] (1) Instruments and reagents

[0032] American Thermo Trace GC Ultra gas chromatograph with hydrogen flame detector (FID); Japanese FrontierPY-2020iD double-click vertical micro-furnace cracker.

[0033] Buy local Fritillaria, Fritillaria Chuan, and Pingbei decoction pieces from pharmacies in Zhejiang, Sichuan, Jilin, etc., remove impurities such as roots and hairs that are visible to the naked eye, grind them, pass through a 60-100 mesh sieve, and make Fritillaria powder for later use. The sample list is shown in Table 1.

[0034]

[0035] (2) Experimental method

[0036]Accurately weigh about 0.3 mg of Zhe Fritillaria (ZB1) sample powder, put it into a sample cup, fix it on the injection rod, and put it into the cracker installed above the GC inlet. At this time, the sample is at room temperature. After the temperature of the cracker reaches the appropriate temperature (400°C, 450°C, 500°C), press the s...

Embodiment 2

[0042] The pyrolysis gas chromatographic analysis of different Fritillaria species of embodiment 2

[0043] American Thermo Trace GC Ultra gas chromatograph with hydrogen flame detector (FID); Japanese FrontierPY-2020iD double-click vertical micro-furnace cracker.

[0044] Gas chromatographic conditions: UA-CW capillary column (30m x 0.25mm i.d.x 0.25um, PEG20), heating program: initial temperature 40°C, rise to 90°C at a rate of 20°C / min, then rise to 90°C at a rate of 10°C / min 250°C, hold for 5min; inlet temperature is 250°C, detector temperature is 250°C, split ratio 30:1; carrier gas: nitrogen, flow rate 1.0mL / min.

[0045] Cracker conditions: cracking furnace temperature: 450°C; interface temperature between cracker and gas chromatograph: 250°C.

[0046] Accurately weigh 0.3 mg of Zhe Fritillaria (ZB1), Chuan Fritillaria (CB1), and Flat Fritillaria (PB1) prepared according to the method of Example 1 respectively, put them into sample cups, fix them on the sampling rod, a...

Embodiment 3

[0049] The investigation of embodiment 3 reproducibility

[0050] American Thermo Trace GC Ultra gas chromatograph with hydrogen flame detector (FID); Japanese FrontierPY-2020iD double-click vertical micro-furnace cracker.

[0051] Gas chromatographic conditions: UA-CW capillary column (30m x 0.25mm i.d.x 0.25um, PEG20), heating program: initial temperature 40°C, rise to 90°C at a rate of 20°C / min, then rise to 90°C at a rate of 10°C / min 250°C, hold for 5min; inlet temperature is 250°C, detector temperature is 250°C, split ratio 30:1; carrier gas: nitrogen, flow rate 1.0mL / min.

[0052] Cracker conditions: cracking furnace temperature: 450°C; interface temperature between cracker and gas chromatograph: 250°C.

[0053] Accurately weigh 0.3 mg of 5 parts of Fritillaria (ZB1) samples prepared by the method of Example 1 respectively and put them into the sample cup, fix them behind the sample rod, and pack into the cracker installed on the top of the GC sample inlet. At this time...

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Abstract

The invention discloses a method for identifying fritillaria thunbergii, fritillaria cirrhosa and fritillaria ussuriensis with pyrolysis-gas chromatography fingerprints. The method comprises the following steps: putting the known fritillaria thunbergii, fritillaria cirrhosa and fritillaria ussuriensis powder into a cracker, connecting the cracker to an injection port of a gas chromatograph, injecting samples when the temperature of the cracker reaches 400 to 500 DEG C, obtaining a fritillaria pyrogram by chromatogram column separation, selecting characteristic peaks to obtain characteristic components, establishing a fingerprint database, and then classifying the samples into fritillaria thunbergii, fritillaria cirrhosa or fritillaria ussuriensis by statistical analysis. The pyrolysis-gaschromatography adopts direct injection of solid samples without a solvent, so that the operation is simple and environment-friendly; and the development of pyrolysis chromatography can effectively save the experimental time and simplify the experimental steps.

Description

(1) Technical field [0001] The invention relates to a method for distinguishing Fritillaria chinensis, Fritillaria sichuanensis and Fritillaria chinensis and Fritillaria chinensis, in particular to a method for distinguishing Fritillaria chinensis, Fritillaria sichuanensis and Fritillaria chinensis and Fritillaria chinensis in combination with fingerprints. (2) Background technology [0002] The traditional Chinese medicine Fritillaria is the dried bulb of certain plants of the Liliaceae Fritillaria (Fritillaria), which has the effects of clearing away heat and nourishing the lungs, reducing phlegm and relieving cough. traditional Chinese medicine. According to different functions, fritillary medicinal materials have formed two major systems, "Chuanbei" and "Zhebei". Chuanbei is the most valuable type of fritillaria, and it mainly grows in the Hengduan mountainous area, including the Liliaceae plant Fritillaria fritillaria. cirrhosa D.Don, Fritillaria unibracteata Hsiao et ...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/02G01N30/06G01N30/54
CPCG01N30/02G01N30/06G01N30/54G01N30/88G01N2030/025G01N2030/062G01N2030/8809
Inventor 刘会君陈雪黄忠平黄翌磊王丽丽
Owner ZHEJIANG UNIV OF TECH
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