CN108051535A - A kind of method of UPLC-MS-MS rapid screenings Sculellaria barbata different sources otherness - Google Patents
A kind of method of UPLC-MS-MS rapid screenings Sculellaria barbata different sources otherness Download PDFInfo
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- CN108051535A CN108051535A CN201711404173.XA CN201711404173A CN108051535A CN 108051535 A CN108051535 A CN 108051535A CN 201711404173 A CN201711404173 A CN 201711404173A CN 108051535 A CN108051535 A CN 108051535A
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/8813—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample biological materials
Abstract
The invention discloses a kind of method of UPLC MS MS rapid screenings Sculellaria barbata different sources otherness, including：（1）Different sources, the Sculellaria barbata medicinal material of different batches are collected, standard decoction sample is made；（2）Sample is entered UPLC MS MS systems to analyze, obtains corresponding mass spectrometric data；（3）The data of acquired original are introduced directly into Compound Discoverer2.1, carry out data analysis；（4）Using the correction chromatographic peak drift of Dynamic Programming calculating method, align chromatographic peak, and the substance for being closer to retention time using closest clustering method is registered as a compound；（5）The substance of sample room otherness is calculated using variance analysis, determines the otherness of different sources Sculellaria barbata.The output of compound Information in Mass Spectra is original document by the present invention, it is not required to be converted into extended formatting, it can be introduced directly into and search for compound into Compound Discoverer2.1 storehouses, this method can realize otherness compound present in quick lock in Sculellaria barbata sample, and measure is quickly analyzed suitable for high-volume sample.
Description
Technical field
The invention belongs to traditional Chinese medicine ingredients studying technological domains, and in particular to a kind of UPLC-MS-MS rapid screenings Sculellaria barbata is not
With the method for place of production otherness.
Background technology
Sculellaria barbata is labiate Sculellaria barbataScutellaria barbataThe drying herb of D.Don, main product is in half
The ground such as branch lotus main product Hebei, Henan, Shanxi, Shaanxi, Anhui.The active ingredient of Chinese medicine is due to factors such as region, weather, kinds
Difference, even if by same Chinese medicine, also can there are the differences of active ingredient.Therefore, to the medicinal materials of the same race of different sources into
Row screening has important practical significance for promoting Quality Evaluation of Chinese Medicinal.
At present, mainly there are HPLC, IR, NIR, TLC etc. to the discrimination method in the Chinese medicine place of production, exist in these methods a large amount of
False positive and Problem of False Negative, when causing to be analyzed using these methods, important material information may be missed, and then led
Cause filtered out otherness substance can not Efficient Characterization group differences, the Chinese medical herb of the same race for determining different sources is brought
It is difficult.
The content of the invention
To solve the above problems, it is an object of the invention to provide a kind of UPLC-MS-MS quick, that accuracy is high is quick
The method of examination Sculellaria barbata different sources otherness.
The present invention is to be achieved through the following technical solutions：
A kind of method of UPLC-MS-MS rapid screenings Sculellaria barbata different sources otherness, comprises the following steps：
（1）The Sculellaria barbata medicinal material of different sources to be distinguished, different batches is collected, by the different batches Sculellaria barbata medicine in the identical place of production
Material is divided into one group, and every group of Sculellaria barbata medicinal material is made Sculellaria barbata standard decoction sample, crushes, and crosses 60 mesh sieves, is protected from light at -20 DEG C
It preserves；
（2）Take step（1）Sculellaria barbata standard decoction sample each 0.5g, it is accurately weighed, put in conical flask with cover, precision adds in
50-80% ethyl alcohol 25ml, weighed weight are heated to reflux 20-40 minutes, let cool, then weighed weight, are supplied and subtracted with 50-80% ethyl alcohol
The weight of mistake, shakes up, and filtration takes subsequent filtrate, is prepared into test solution, subsequently enters UPLC-MS-MS systems and analyzed,
Obtain the corresponding mass spectrometric data of each sample；
（3）By step（2）The data of acquisition are directed into Compound Discoverer2.1, data analysis are carried out, for each
Sample carries out chromatographic peak extraction and Information in Mass Spectra characterization；
（4）The sample for selecting substance chromatographic peak quantity most is as reference sample, using between Dynamic Programming calculating method correcting sample
Chromatographic peak drift, alignment belonged to the chromatographic peak of same substance, then more connect retention time using closest clustering method
Near substance is registered as a compound, finally establishes the accreditation charts of a sample and chromatographic peak；After external standard corrects,
For subsequent analysis；
（5）The substance of sample room otherness is calculated using variance analysis, confidence level threshold is set as 0.05, and confidence level is small
Substance in 0.05 is regarded as otherness compound, and the original document of the Information in Mass Spectra of all differences substance is importing directly into
Compound Discoverer2.1 are matched in storehouse, determine the structure of matter, so as to obtain otherness substance；Then color is passed through
The peak area of spectrum and the mass number of the corresponding quasi-molecular ion peak of appearance retention time determine the otherness of different sources Sculellaria barbata.
Wherein, step（1）Sculellaria barbata standard decoction sample be basis《Chinese medicinal granule quality control and standard formulation
Technology requirement》In " standard decoction preparation " item guideline requirement prepare.The present invention is to Sculellaria barbata standard decoction sample preparation
Maximum effect factor immersion way in technique is investigated, and compares cold water soak and boiling water feeds intake two kinds of technology modes, tool
Body method is as follows：
A, warm water immersion process：
Sculellaria barbata medicine materical crude slice 100g is taken, adds in 13 times of amount warm water, after impregnating 30 minutes, intense fire（Power 500W）It is heated to boiling, slow boiling
（Power 200W）It keeps slightly boiling 20 minutes, is filtered while hot with 350 mesh screens, filtrate is cooled down rapidly with cold water；Second of decoction adds
10 times of amount water, intense fire are heated to boiling, and slow boiling keeps slightly boiling 15 minutes, is filtered while hot with 350 mesh screens, filtrate is cold rapidly with cold water
But, filtrate twice is merged, freeze-drying obtains Sculellaria barbata standard decoction sample 1.
B, boiling water feeding method：
Sculellaria barbata medicine materical crude slice 100g is taken, is put into the 13 times of amount water boiled, intense fire（Power 500W）After boiling, slow boiling（Power
200W）It keeps slightly boiling 20 minutes, is filtered while hot with 350 mesh screens, filtrate is cooled down rapidly with cold water；Second of decoction plus 10 times of amounts
Water, intense fire are heated to boiling, and slow boiling keeps slightly boiling 15 minutes, is filtered while hot with 350 mesh screens, and filtrate is cooled down rapidly with cold water, closes
And filtrate, freeze-drying obtain Sculellaria barbata standard decoction sample 2 twice.
Comparative measurements warm water, boiling water Sculellaria barbata standard decoction paste-forming rate, Content Measurement of Scutellarin and the scutellarin rate of transform,
Experimental result see the table below.
Different decocting processes influence result to Sculellaria barbata standard decoction parameter
The experimental results showed that Sculellaria barbata standard decoction has no too big difference in 30 minutes using temperature leaching with the paste-forming rate that boiling water feeds intake
Not, but Content Measurement of Scutellarin and the scutellarin rate of transform, boiling water charging technology are significantly larger than temperature 30 minutes technique of leaching, and reason may
It is Sculellaria barbata during warm water impregnates, there are enzyme degradation reactions for scutellarin.Therefore, in raising Sculellaria barbata standard decoction
The transfer of scutellarin, the decocting process of Sculellaria barbata standard decoction is preferably boiling water feeding mode.
Preferably, step（1）In, the Sculellaria barbata standard decoction sample obtains by the following method：
Sculellaria barbata medicinal material is taken, is added water to cook twice, 10-15 times boiled is put into for the first time and measures in water, intense fire（500w）Heating
To boiling, slow boiling（300w）It keeps slightly boiling 15-30 minutes, is filtered while hot with 350 mesh screens, filtrate is cooled down rapidly with cold water；Second
Secondary decoction adds 8-12 times and measures water, intense fire（500w）It is heated to boiling, slow boiling（300w）Slightly boiling is kept 10-20 minutes, with 350 mesh screens
Filter while hot, filtrate is cooled down rapidly with cold water, merges filtrate twice, be freeze-dried to get.
The preparation method of the Sculellaria barbata standard decoction sample of the present invention meets the prepared slices of Chinese crude drugs of traditional Chinese medicine theory high praise
The viewpoint being used as medicine with decoction avoids the security wind brought using organic solvent as solvent using drinking water as extraction solvent
Danger can preferably retain the information of majority of compounds in Sculellaria barbata, more meet Chinese medicine Clinical practice custom, and obtain Sculellaria barbata
The information content bigger of sample improves the accuracy and reappearance of detection.
Pass through the optimization of solvent strength and extraction time, it is preferred that step（2）Specially：Take step（1）Sculellaria barbata mark
Quasi- each 0.5g of decoction sample, it is accurately weighed, it puts in conical flask with cover, precision adds in 70% ethyl alcohol 25ml, and weighed weight heats back
Stream 30 minutes, lets cool, then weighed weight, and the weight of less loss is supplied with 70% ethyl alcohol, is shaken up, and filters, takes subsequent filtrate, is made for examination
Product solution subsequently enters UPLC-MS-MS systems and is analyzed, and obtains the corresponding spectra count of each Sculellaria barbata standard decoction sample
According to.
Preferably, step（2）In, the analysis condition of the UPLC-MS-MS systems is：
Chromatographic condition：C18 chromatographic columns, using 0.2% formic acid-water as mobile phase A, chromatography methanol is Mobile phase B gradient elution such as following table
It is shown；Flow velocity：0.4ml/min；Column temperature is 30 DEG C；Detection wavelength is 335nm；Number of theoretical plate should not be low by the calculating of scutellarin peak
In 1500；
Mass Spectrometry Conditions：Using multiple-reaction monitoring MRM scan patterns, electric spray ion source ESI is gathered under negative ion mode；Data
Acquisition range m/z100~1000；Source parameters:Capillary voltage:3 kV, ion source temperature:It 150 DEG C, takes off
Solvent temperature degree:350 DEG C, 60 Lh of atomization gas flow velocity-1, 600 Lh of Desolvention gas velocity-1;Collision energy: 10
~40 V；Sweep time：5.00 -35.00min；Orifice potential is 25V；
The detection ion pair of scutellarin analyte：m/z 461.08/285.05、m/z461.08/194.04；Sweep time：
5.00 -8.00min；Residence time：0.005；Orifice potential：25V；Impact energy：40V；
The detection ion pair of apiolin analyte：m/z 269.24/151.02、m/z269.24/117.05；Sweep time：7.00
-12.00min；Residence time：0.005；Orifice potential：25V；Impact energy：40V.
Compared with prior art, the present invention it has the advantages that：
（1）For the first time using UPLC-MS-MS rapid screening Sculellaria barbata different sources othernesses, this method has quick, accurate the present invention
Really, the advantages that stablizing；
（2）The output of compound Information in Mass Spectra is original document by the present invention, and this document is not required to be converted into extended formatting, can directly lead
Enter into Compound Discoverer2.1 storehouses and search for compound, this method can be realized deposits in quick lock in Chinese medicine sample
Otherness compound, quickly analyze measure suitable for high-volume sample；
（3）The present invention, as test sample, is studied using the standard decoction sample of Sculellaria barbata medicinal material for water-soluble extractive
Analysis is investigated by the optimization of extraction process, and research draws the preparation process of Sculellaria barbata standard soup；It is established with reference to the present invention
The screening method of Sculellaria barbata different sources can be promoted and applied and selected in the raw material of Sculellaria barbata granule product and its related preparations
In preparation process.
Description of the drawings
Fig. 1 is the high performance liquid chromatography comparison chart of the Sculellaria barbata standard decoction sample in the Sichuan place of production and the Hunan place of production；
Fig. 2 is the high-efficient liquid phase chromatogram and TIC figures of scutellarin and the mixed mark reference substance of two kinds of apiolin；
Fig. 3 is the high-efficient liquid phase chromatogram of the Sculellaria barbata standard decoction sample in the Sichuan place of production and TIC figures；
Fig. 4 is the high-efficient liquid phase chromatogram of the Sculellaria barbata standard decoction sample in the Hunan place of production and TIC figures；
Fig. 5 is the PCA figures of the Sculellaria barbata standard decoction sample in the Sichuan place of production and the Hunan place of production.
Specific embodiment
It is further illustrated the present invention below by specific embodiment, following embodiment is the specific embodiment party of the present invention
Formula, but embodiments of the present invention and from the limitation of following embodiments.
Embodiment 1
A kind of method of UPLC-MS-MS rapid screenings Sculellaria barbata different sources otherness, comprises the following steps：
（1）Totally 30 Sculellaria barbata medicinal materials are collected from Hunan and 2, Sichuan area, by the Sculellaria barbata medicine of the different batches in the identical place of production
Material is divided into one group, and every group of Sculellaria barbata medicinal material is made Sculellaria barbata standard decoction sample, is freeze-dried, and crushes, and crosses 60 mesh sieves, in-
It is kept in dark place at 20 DEG C；
Wherein, Sculellaria barbata standard decoction sample obtains by the following method：Sculellaria barbata medicinal material is taken, is added water to cook twice, for the first time
It puts into the 13 times of amount water boiled, intense fire（500w）It is heated to boiling, slow boiling（300w）Slightly boiling is kept 20 minutes, with 350 mesh sieves
Net filters while hot, and filtrate is cooled down rapidly with cold water；Second of decoction plus 10 times of amount water, intense fire（500w）It is heated to boiling, slow boiling
（300w）It keeps slightly boiling 15 minutes, is filtered while hot with 350 mesh screens, filtrate is cooled down rapidly with cold water, merges filtrate twice, freezing
It is dry to get；
（2）Take step（1）Sculellaria barbata standard decoction sample each 0.5g, it is accurately weighed, put in conical flask with cover, precision adds in
70% ethyl alcohol 25ml, weighed weight are heated to reflux 30 minutes, let cool, then weighed weight, and the weight of less loss is supplied with 70% ethyl alcohol,
It shakes up, filters, take subsequent filtrate, test solution is made, subsequently enters UPLC-MS-MS systems and is analyzed, obtain each half
The corresponding mass spectrometric data of lotus standard decoction sample；
Wherein, the analysis condition of the UPLC-MS-MS systems is：
Chromatographic condition：C18 chromatographic columns, using 0.2% formic acid-water as mobile phase A, chromatography methanol is Mobile phase B, and gradient elution is as follows
Shown in table；Flow velocity：0.4ml/min；Column temperature is 30 DEG C；Detection wavelength is 335nm；Number of theoretical plate should not by the calculating of scutellarin peak
Less than 1500；
Mass Spectrometry Conditions：Using multiple-reaction monitoring MRM scan patterns, electric spray ion source ESI is gathered under negative ion mode；Data
Acquisition range m/z100~1000；Source parameters:Capillary voltage:3 kV, ion source temperature:It 150 DEG C, takes off
Solvent temperature degree:350 DEG C, 60 Lh of atomization gas flow velocity-1, 600 Lh of Desolvention gas velocity-1;Collision energy: 10
~40 V；Sweep time：5.00 -35.00min；Orifice potential is 25V；
The detection ion pair of scutellarin analyte：m/z 461.08/285.05、m/z461.08/194.04；Sweep time：
5.00 -8.00min；Residence time：0.005；Orifice potential：25V；Impact energy：40V；
The detection ion pair of apiolin analyte：m/z 269.24/151.02、m/z269.24/117.05；Sweep time：7.00
-12.00min；Residence time：0.005；Orifice potential：25V；Impact energy：40V；
（3）By step（2）The data of each acquired original of the Sculellaria barbata standard decoction sample after UPLC-MS-MS is analyzed are straight
Connect and be directed into Compound Discoverer2.1, then carry out data analysis, for each sample carry out chromatographic peak extraction and
Information in Mass Spectra characterizes；
（4）The sample for selecting substance chromatographic peak quantity most is as reference sample, using between Dynamic Programming calculating method correcting sample
Chromatographic peak drift, alignment belonged to the chromatographic peak of same substance, then more connect retention time using closest clustering method
Near substance is registered as a compound, finally establishes the accreditation charts of a sample and chromatographic peak；After external standard corrects,
For subsequent analysis；Such as Fig. 1-4, the chromatogram in the Sichuan place of production and Hunan place of production Sculellaria barbata standard decoction and total ion are shown
Flow graph（TIC）；
（5）Utilize principal component analysis（PCA）To the total ion current of the Sculellaria barbata standard decoction sample in the Sichuan place of production and the Hunan place of production
Diagram data is analyzed, the results show（Such as Fig. 5）, every group of data are gathered in respective 95% confidence limit ellipse figure, and two groups
Data can be kept completely separate, and illustrated the Sculellaria barbata standard decoction sample in the Sichuan place of production and the Hunan place of production and can completely be divided
From.The substance of sample room otherness is calculated using variance analysis, confidence level threshold is set as 0.05, confidence level is less than
0.05 substance is regarded as otherness compound, and the original document of the Information in Mass Spectra of all differences substance is importing directly into
Compound Discoverer2.1 are matched in storehouse, determine the structure of matter, so as to obtain otherness substance, then pass through color
The peak area of spectrum and the mass number of the corresponding quasi-molecular ion peak of appearance retention time determine the otherness of different sources Sculellaria barbata.
The results show that the Sculellaria barbata standard decoction sample in the Hunan place of production is in retention time 9.35, relative retention time 0.38（With apiolin
Retention time is standard）For the peculiar peak of following structural compounds, molecular weight 432.33；
And the Sculellaria barbata standard decoction sample in the Sichuan place of production is in retention time 9.05min, relative retention time 0.37（With apiolin
Retention time is standard）It is apiolin -7- O- glucuronic acids by interpretation of mass spectra, molecular weight 446.36, structural formula is such as
Shown in lower：
。
Claims (4)
- A kind of 1. method of UPLC-MS-MS rapid screenings Sculellaria barbata different sources otherness, which is characterized in that including following step Suddenly：（1）The Sculellaria barbata medicinal material of different sources to be distinguished, different batches is collected, by the different batches Sculellaria barbata medicine in the identical place of production Material is divided into one group, and every group of Sculellaria barbata medicinal material is made Sculellaria barbata standard decoction sample, crushes, and crosses 60 mesh sieves, is protected from light at -20 DEG C It preserves；（2）Take step（1）Sculellaria barbata standard decoction sample each 0.5g, it is accurately weighed, put in conical flask with cover, precision adds in 50-80% ethyl alcohol 25ml, weighed weight are heated to reflux 20-40 minutes, let cool, then weighed weight, are supplied and subtracted with 50-80% ethyl alcohol The weight of mistake, shakes up, and filtration takes subsequent filtrate, and test solution is made, subsequently enters UPLC-MS-MS systems and is analyzed, obtained To the corresponding mass spectrometric data of each Sculellaria barbata standard decoction sample；（3）By step（2）The data of acquisition are introduced directly into Compound Discoverer2.1, then carry out data analysis, Chromatographic peak extraction and Information in Mass Spectra characterization are carried out for each sample；（4）The sample for selecting substance chromatographic peak quantity most is as reference sample, using between Dynamic Programming calculating method correcting sample Chromatographic peak drift, alignment belonged to the chromatographic peak of same substance, then more connect retention time using closest clustering method Near substance is registered as a compound, finally establishes the accreditation charts of a sample and chromatographic peak；After external standard corrects, For subsequent analysis；（5）The substance of sample room otherness is calculated using variance analysis, confidence level threshold is set as 0.05, and confidence level is small Substance in 0.05 is regarded as otherness compound, and the original document of the Information in Mass Spectra of all differences substance is importing directly into Compound Discoverer2.1 are matched in storehouse, determine the structure of matter, so as to obtain otherness substance；Then color is passed through The peak area of spectrum and the mass number of the corresponding quasi-molecular ion peak of appearance retention time determine the otherness of different sources Sculellaria barbata.
- 2. a kind of method of UPLC-MS-MS rapid screenings Sculellaria barbata different sources otherness according to claim 1, It is characterized in that, step（1）In, the Sculellaria barbata standard decoction sample obtains by the following method：Sculellaria barbata medicinal material is taken, is added water to cook twice, 10-15 times boiled is put into for the first time and measures in water, intense fire is heated to boiling, text Fire keeps slightly boiling 15-30 minutes, is filtered while hot with 350 mesh screens, filtrate is cooled down rapidly with cold water；Second of decoction adds 8-12 times Water is measured, intense fire is heated to boiling, and slow boiling keeps slightly boiling 10-20 minutes, is filtered while hot with 350 mesh screens, filtrate is cold rapidly with cold water But, merge filtrate twice, be freeze-dried to get.
- 3. a kind of method of UPLC-MS-MS rapid screenings Sculellaria barbata different sources otherness according to claim 1, It is characterized in that, step（2）Specially：By step（1）Obtained all Sculellaria barbata standard decoction sample 0.5g, it is accurately weighed, it puts In conical flask with cover, precision adds in 70% ethyl alcohol 25ml, and weighed weight is heated to reflux 30 minutes, lets cool, then weighed weight, uses 70% ethyl alcohol supplies the weight of less loss, shakes up, filtration, take subsequent filtrate, be configured to solution, subsequently enter UPLC-MS-MS systems into Row analysis, obtains the corresponding mass spectrometric data of each Sculellaria barbata standard decoction sample.
- 4. a kind of method of UPLC-MS-MS rapid screenings Sculellaria barbata different sources otherness according to claim 1, It is specialSign is, step（2）In, the analysis condition of the UPLC-MS-MS systems is：Chromatographic condition：C18 chromatographic columns, using 0.2% formic acid-water as mobile phase A, chromatography methanol is Mobile phase B, and gradient elution is as follows Shown in table；Flow velocity：0.4ml/min；Column temperature is 30 DEG C；Detection wavelength is 335nm；Number of theoretical plate should not by the calculating of scutellarin peak Less than 1500；Mass Spectrometry Conditions：Using multiple-reaction monitoring MRM scan patterns, electric spray ion source ESI is gathered under negative ion mode；Data acquisition range M/z100~1000；Source parameters:Capillary voltage:3 kV, ion source temperature:150 DEG C, desolventizing temperature Degree:350 DEG C, 60 Lh of atomization gas flow velocity-1, 600 Lh of Desolvention gas velocity-1;Collision energy:10~40 V；It sweeps Retouch the time：5.00 -35.00min；Orifice potential is 25V；The detection ion pair of scutellarin analyte：m/z 461.08/285.05、m/z461.08/194.04；Sweep time： 5.00 -8.00min；Residence time：0.005；Orifice potential：25V；Impact energy：40V；The detection ion pair of apiolin analyte：m/z 269.24/151.02、m/z269.24/117.05；Sweep time：7.00 -12.00min；Residence time：0.005；Orifice potential：25V；Impact energy：40V.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114113348A (en) * | 2020-08-26 | 2022-03-01 | 国药集团同济堂（贵州）制药有限公司 | Preparation method, characteristic spectrum and content determination method of rose standard decoction |
| CN114113348B (en) * | 2020-08-26 | 2023-10-17 | 国药集团同济堂（贵州）制药有限公司 | Preparation method of standard rose decoction, characteristic spectrum and content determination method |
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