CN111650304A - Method for rapidly screening sulphur-smoked flos farfarae - Google Patents
Method for rapidly screening sulphur-smoked flos farfarae Download PDFInfo
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- CN111650304A CN111650304A CN202010609773.5A CN202010609773A CN111650304A CN 111650304 A CN111650304 A CN 111650304A CN 202010609773 A CN202010609773 A CN 202010609773A CN 111650304 A CN111650304 A CN 111650304A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G01N30/72—Mass spectrometers
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Abstract
The invention belongs to the technical field of detection of traditional Chinese medicinal materials, and particularly relates to a method for rapidly screening sulphur-smoked flos farfarae. The method comprises the steps of pulverizing and sieving the coltsfoot flower medicinal materials to be distinguished to prepare a sample to be tested, adding a proper amount of sample powder into methanol, carrying out ultrasonic extraction to obtain a sample solution to be tested, and analyzing by using a liquid chromatography-mass spectrometry technology; screening whether the test sample contains any one or more of characteristic diagnostic ions according to the mass spectrum data of the test sample and through the excimer ion peak and the secondary mass spectrum information of the target product; if the characteristic diagnosis ions are detected, the common coltsfoot flower is fumigated by sulfur; if the characteristic diagnostic ion is not detected, the flos farfarae is not sulfited. The method for screening the flos farfarae sulfitation can quickly and accurately identify whether the flos farfarae is sulfitation or not. Even if SO2The residue meets the relevant regulations of Chinese pharmacopoeiaThe diagnosis ions determined by the invention can also accurately identify whether the coltsfoot flower medicinal material is subjected to sulfitation.
Description
Technical Field
The invention belongs to the technical field of detection of traditional Chinese medicinal materials, and particularly relates to a method for rapidly screening sulphur-smoked flos farfarae.
Background
Sulfur fumigation is a traditional method for processing and maintaining traditional Chinese medicinal materials, and is currently used for processing various medicinal materials, such as sulfur-fumigated ginger, sulfur-fumigated bighead atractylodes rhizome and the like. SO generated by sulfur combustion in the sulfitation process2Is a strong reducing agent, and can bleach and prevent certain chemical reactions of discolorationThe reaction takes place, drying is accelerated, and most bacteria can be killed.
Flos Farfarae is dry bud of flos Farfarae (Tussilago farfara L.) of Compositae, has warm, pungent and slightly bitter properties, has effects of moistening lung, descending qi, relieving cough and eliminating phlegm, and is commonly used for treating overstrain cough, hemoptysis, asthma, excessive phlegm, and new and long-term cough. Research shows that the sesquiterpenoids and phenylpropanoids are the main chemical components in the flos farfarae and the main components of the flos farae for exerting the drug effect. The traditional drying mode of the flos farfarae is shade drying, and at present, drying is mostly adopted. In the drying process, sulfur is adopted by illegal vendors for fumigation.
SO generated by sulfur fumigation in Chinese pharmacopoeia2And controlling the residual quantity. But SO2The volatile gas may decrease with storage time and fall below the detection limit. The literature reports that chemical components of medicinal materials can be changed after sulfur fumigation, and the change of the chemical components can influence the effectiveness and safety of the medicinal materials. Therefore, even after the stoving, the medicinal material SO2The residual quantity is qualified, but the internal chemical composition of the residual quantity is changed, namely the residual quantity is only based on SO2The residue cannot be used to determine whether the herb has been subjected to sulfitation.
Disclosure of Invention
Aiming at the problems, the invention provides a method for rapidly screening sulphur-smoked common coltsfoot flowers.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for rapidly screening sulphur smoked flos farfarae comprises the following steps:
step 1, pulverizing and sieving flos farfarae medicinal materials to be distinguished to prepare a sample to be tested, adding a proper amount of sample powder into methanol, performing ultrasonic extraction to obtain a sample solution to be tested, and analyzing by using a liquid chromatography-mass spectrometry technology;
step 2, screening whether the sample contains any one or more of characteristic diagnostic ions or not according to the mass spectrum data of the sample to be tested and through the excimer ion peak and the secondary mass spectrum information of the target product;
step 3, if the characteristic diagnosis ions are detected, the common coltsfoot flower is fumigated by sulfur; if the characteristic diagnostic ion is not detected, the flos farfarae is not sulfited.
Further, the methanol is 10-20 times of the sample to be tested; the ultrasonic extraction time is 20-40 min.
Still further, the methanol is 20 times of the amount of the test sample; the ultrasonic extraction time is 20 min.
Further, the characteristic diagnostic ions include: a sulfate-formed product of monocaffeoylquinic acid, a sulfate-formed product of dicaffeoylquinic acid, and a sulfurous acid addition product of dicaffeoylquinic acid.
Still further, the mono-caffeoyl quinic acid sulfation product: the peak of the quasi-molecular ion is 433.0446[ M-H]-Secondary fragments are 415.0340, 387.0391, 353.0878, 258.9917, 240.9812, 191.0561, 179.0349.
Still further, the dicaffeoylquinic acid sulfation product: the peak of the quasi-molecular ion is 595.0763[ M-H]-Secondary fragments are 577.0657, 549.0708, 515.1194, 353.0878, 258.9917, 240.9812, 191.0561, 179.0349.
Still further, the dicaffeoylquinic acid sulfurous acid addition product: the peak of the quasi-molecular ion is 597.0919[ M-H]-Secondary fragments are 515.1194, 353.0878, 191.0561, 179.0349.
Compared with the prior art, the invention has the following advantages:
the method for screening whether the flos farfarae is sulfitation or not is rapidly screened by using high performance liquid chromatography-high resolution mass spectrometry, and the established flos farfarae sulfitation screening method can rapidly and accurately identify whether the flos farfarae is sulfitation or not. Even if SO2The residue accords with the relevant regulations of Chinese pharmacopoeia, and the diagnosis ions determined by the invention can also accurately identify whether the coltsfoot flower medicinal material is subjected to sulfitation.
Detailed Description
The present invention will be described in further detail with reference to specific examples, which are provided only for the purpose of the present invention and are not intended to limit the scope of the present invention. Further, it is to be understood that various changes or modifications may be made by one skilled in the art after reading the disclosure of the present invention, and such equivalents are also within the scope of the invention as defined in the appended claims.
Example 1
Method for rapidly screening sulphur-smoked flos farfarae
Pulverizing unvulcanized flos Farfarae and sulfited flos Farfarae in different producing areas, and sieving to obtain sample; taking a proper amount of a sample to be tested, precisely weighing, placing in a conical flask with a plug, precisely adding 20 times of methanol, performing ultrasonic treatment for 20min, filtering, taking a subsequent filtrate to obtain a sample solution to be tested, and analyzing by using a liquid chromatography-mass spectrometry method;
wherein, the analysis conditions of the ultra-high performance liquid chromatography tandem high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) are as follows:
chromatographic conditions are as follows: waters Acquity UHPLC HSS T3 chromatography column (2.1 mm. times.100 mm,1.8 μm); taking 0.1% formic acid-acetonitrile as a mobile phase A and 0.1% formic acid-water as a mobile phase B; flow rate: 0.3 mL/min; the column temperature was 40 ℃; the sample injection amount is 3 mu L; gradient elution is shown in table 1:
TABLE 1
Mass spectrum conditions: ionization mode: ESI (-); the detection mode is as follows: full scanning; spraying voltage: 3.5 kV;
flow rate of sheath gas: 45 psi; flow rate of auxiliary gas: 15 psi; capillary temperature: 320 ℃; probe card
Temperature of the warmer: 320 ℃; scanning range: 80-1200m/z, mass resolution: 70000
According to the mass spectrum data of the sample to be tested, the quasi-molecular ion peak and the secondary mass spectrum information of the target product in the sample are screened, and the screening results of 10 batches of non-sulfitation tussilago farfara and 6 batches of sulfitation tussilago fara are shown in table 2.
Extraction of the excimer ion Peak [ M-H]-433.0446, whose secondary mass spectral fragments include 415.0340, 387.0391, 353.0878, 258.9917, 240.9812, 191.0561, 179.0349, the compound was confirmed to be a monocaffeoylquinic acid sulfation product; the quasi-molecular ion peak of 595.0763M-H is extracted by the same method]-The secondary fragment is 577.0657, 549.0708, 515.1194, 353.0878, 258.9917, 240.9812, 191.0561 and 179.0349, the compound is a sulfate product of dicaffeoylquinic acid; the peak of extracted quasi-molecular ion is 597.0919[ M-H]-When the secondary fragments are 515.1194, 353.0878, 191.0561 and 179.0349; the compound is a sulfurous acid addition product of dicaffeoylquinic acid.
TABLE 2
As can be seen from table 2, two or more of the mono-caffeoyl quinic acid sulfation product, the dicaffeoyl quinic acid sulfation product and the dicaffeoyl quinic acid sulfurous acid addition product can be detected in 6 batches of sulfitation flos farfarfarae, and any one of the mono-caffeoyl quinic acid sulfation product, the dicaffeoyl quinic acid sulfation product and the dicaffeoyl quinic acid sulfurous acid addition product is not detected in 10 batches of non-sulfitation flos farae, which indicates that the accuracy of the established method for sulfur fumigation screening of flos farfarae reaches 100%.
Those skilled in the art will appreciate that the invention may be practiced without these specific details. Although illustrative embodiments of the present invention have been described above to facilitate the understanding of the present invention by those skilled in the art, it should be understood that the present invention is not limited to the scope of the embodiments, and various changes may be made apparent to those skilled in the art as long as they are within the spirit and scope of the present invention as defined and defined by the appended claims, and all matters of the invention which utilize the inventive concepts are protected.
Claims (7)
1. A method for rapidly screening sulphur-fumigated flos farfarae is characterized by comprising the following steps: the method comprises the following steps:
step 1, pulverizing and sieving flos farfarae medicinal materials to be distinguished to prepare a sample to be tested, adding a proper amount of sample powder into methanol, performing ultrasonic extraction to obtain a sample solution to be tested, and analyzing by using a liquid chromatography-mass spectrometry technology;
step 2, screening whether the sample contains any one or more of characteristic diagnostic ions or not according to the mass spectrum data of the sample to be tested and through the excimer ion peak and the secondary mass spectrum information of the target product;
step 3, if the characteristic diagnosis ions are detected, the common coltsfoot flower is fumigated by sulfur; if the characteristic diagnostic ion is not detected, the flos farfarae is not sulfited.
2. The method for rapidly screening the sulfitation coltsfoot flower according to claim 1, wherein the method comprises the following steps: the methanol is 10-20 times of the sample to be tested; the ultrasonic extraction time is 20-40 min.
3. The method for rapidly screening the sulfitation coltsfoot flower according to claim 2, wherein the method comprises the following steps: the methanol is 20 times of the sample to be tested; the ultrasonic extraction time is 20 min.
4. The method for rapidly screening the sulfitation coltsfoot flower according to claim 1, wherein the method comprises the following steps: the characteristic diagnostic ions include: a sulfate-formed product of monocaffeoylquinic acid, a sulfate-formed product of dicaffeoylquinic acid, and a sulfurous acid addition product of dicaffeoylquinic acid.
5. The method for rapidly screening the sulfitation coltsfoot flower according to claim 4, wherein the method comprises the following steps: the mono-caffeoyl quinic acid sulfation product: the peak of the quasi-molecular ion is 433.0446[ M-H]-Secondary fragments are 415.0340, 387.0391, 353.0878, 258.9917, 240.9812, 191.0561, 179.0349.
6. The method for rapidly screening the sulfitation coltsfoot flower according to claim 4, wherein the method comprises the following steps: the di-caffeoyl quinic acid sulfation product: the peak of the quasi-molecular ion is 595.0763[ M-H]-Secondary fragments are 577.0657, 549.0708, 515.1194, 353.0878, 258.9917, 240.9812, 191.0561, 179.0349.
7. The method for rapidly screening the sulfitation coltsfoot flower according to claim 4, wherein the method comprises the following steps: the dicaffeoylquinic acid sulfurous acid addition product: the peak of the quasi-molecular ion is 597.0919[ M-H]-Secondary fragments are 515.1194, 353.0878, 191.0561, 179.0349.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114047264A (en) * | 2021-11-02 | 2022-02-15 | 中国中医科学院中药研究所 | Method for rapidly identifying sulphur-smoked angelica dahurica |
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| CN102495143A (en) * | 2011-07-19 | 2012-06-13 | 上海中医药大学 | Method for rapidly measuring content of three paeoniflorin compounds in white paeony root |
| CN107782836A (en) * | 2017-12-22 | 2018-03-09 | 广东方制药有限公司 | A kind of UPLC MS MS rapid screening sulphuring root of herbaceous peonys and the method for non-sulphuring root of herbaceous peony otherness |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114047264A (en) * | 2021-11-02 | 2022-02-15 | 中国中医科学院中药研究所 | Method for rapidly identifying sulphur-smoked angelica dahurica |
| CN114047264B (en) * | 2021-11-02 | 2023-06-02 | 中国中医科学院中药研究所 | Method for rapidly identifying sulfur-fumigated radix angelicae |
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