CN104359987A - Method for quickly and efficiently dissolving out Chinese herbal medicine ingredients and analyzing and identifying dissolved-out ingredients - Google Patents
Method for quickly and efficiently dissolving out Chinese herbal medicine ingredients and analyzing and identifying dissolved-out ingredients Download PDFInfo
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Abstract
The invention discloses a method for quickly and efficiently dissolving out Chinese herbal medicine ingredients and analyzing and identifying dissolved-out ingredients. The method comprises the following steps: (1) selecting traditional Chinese medicinal materials, and decocting under low pressure to obtain traditional Chinese medicinal material decoction; (2) qualitatively and quantitatively analyzing functional ingredients in the traditional Chinese medicinal material decoction in the step (1) by a high-performance liquid chromatography process in Chinese pharmacopoeia 2010; (3) extracting volatile matters in the traditional Chinese medicinal material decoction in the step (1) by a headspace-solid phase microextraction process, and qualitatively and quantitatively analyzing and identifying the smell active compounds of the volatile matters in the traditional Chinese medicinal material decoction by a gas chromatography-sniffing-mass spectrometry process. The method is high in decoction efficiency and capable of quickly, efficiently, qualitatively and quantitatively detecting the functional ingredients and the smell active compounds in the traditional Chinese medicinal materials.
Description
Technical field
The invention belongs to Chinese crude drug technical field, be specifically related to a kind of rapidly and efficiently stripping of Chinese crude drug composition and the Analysis and Identification method of dissolved element.
Technical background
1, the functional component of Chinese crude drug and volatile ingredient
Chinese crude drug, except containing except abundant basic nutrition element (i.e. protein, fat, carbohydrate, vitamin and mineral matter), also contains miscellaneous material with special efficacy.These effect materials are important substance bases of Chinese crude drug effect performance, determine the quality of Chinese crude drug to a great extent.Traditional Chinese medicinal materials assortment is various, but the difference great disparity of effective constituent between different cultivars, the effective constituent of same kind is also subject to the impact of the many factors such as the place of production, cultural method, growing environment and collecting season, so just seem particularly important for the analysis of Chinese crude drug functional component.Current research concentrates on the content to Chinese crude drug (Different sources, different pharmaceutical position etc.) functional component itself mostly, but less for the report of the functional component determination study in decocting for Chinese herbal medicine liquid dissolved element.Effect material is the material base of herbal cuisine performance, and therefore, we are using the content of effect material in herbal cuisine as criterion.
Volatile ingredient in Chinese crude drug is referred to as volatile oil.It is the oily liquids general name that the class be present in plant has volatility, can be distilled out under water vapor effect.Volatile oil may containing dissimilar tens kinds to one, 200 kind of composition, wherein certain or several composition accounts for larger component.Volatile oil basic composition is aliphatics, aromatic series and terpenoid etc., terpene mainly monoterpene and sequiterpene, and their content is higher usually, but without fragrance, is not the fragrance ingredient of volatile oil; Though some terpene is derivative and aromatic content few containing oxygen, they have the special fragranced of volatile oil and significant biologically active.Also have some other compounds in addition, if: sulfocompound, nitrogenous and sulfocompound are also the ingredients of some volatile oil.In the aroma compound of decocting for Chinese herbal medicine liquid, except comprise some in Chinese medicine with the volatile oil component of aromatic odor, also comprise the aroma compound that some aldehydes, ketones etc. exist in traditional food.Unique local flavor is the key factor that herbal cuisine/Chinese herbal medicine is liked by consumer, and the local flavor of herbal cuisine/Chinese herbal medicine gives the kind of Odor-active compound by its feature and how much determines.
At present, dissolving-out method for functional component in Chinese crude drug and volatile matter adopts traditional normal heating decoction usually, decoct effect and depend on the skill level decocting operator greatly, decoction process is loaded down with trivial details, time of boiling medicine is longer, the feature extracted comparatively up hill and dale in functional component and volatile matter cannot give Odor-active compound at short notice, simultaneously, effect material and smell reactive compound can volatilize with water vapor and lose, decoct big energy-consuming, odor dispersion can cause being full of Chinese medicine taste around, decoction vessel cleaning difficulty, in addition, dissolved element needs before machine extract, concentrate and wait pre-treatment, pre-treatment is general comparatively loaded down with trivial details.In operation, the target component in decoction liquor may be caused damage, cause final measurement result to occur deviation.
2, the analytical approach research of functional component in Chinese crude drug
(1) gas chromatography analysis method (GC): vapor-phase chromatography is one of the most effective means of Analysis of Organic Substances, is widely used in the analysis of Effective Component of Chinese Medicine.Be mainly used in the analysis that boiling point is not too high, Heat stability is good, molecular weight are less than the composition of 400, for other sample, then need to carry out suitable derivatization treatment, to improve its volatility, selectivity or separate condition.
(2) scope of application of high efficiency liquid phase chromatographic analysis method (HPLC): HPLC is comparatively wide, can be used for the sample analyzing higher boiling, thermal sensitivity, macromolecule, is a kind of analytical approach of very effective and blanket Effective Component of Chinese Medicine.Have the principle of absorption in ultraviolet region according to many traditional Chinese medicine ingredients, in high performance liquid chromatography, diode array detector, UV-detector are conventional detecting devices.
(3) thin layer chromatography (TLC): TLC is a kind of microanalysis method, because the method is easy and simple to handle, do not need expensive instrument and equipment, amount of samples is few, detection sensitivity is high, and analysis speed is fast, and separation efficiency is high, just receive in middle 1960s and pay attention to and be widely used greatly, this is that the development of this technology is laid a good foundation.According to the preliminary statistics, the applicable cases of TLC method in the Pharmacopoeia of the People's Republic of China constantly increases, and shows the feature such as easy, quick, practical of the method.
(4) high performance capillary electrophoresis analysis method (HPCE): HPCE is with the highfield produced under high pressure for driving force, and with the quartz capillary of little internal diameter for split tunnel, the difference according to electrophoretic mobility or partition factor between each component realizes being separated.Capillary Electrophoresis is widely used in recent years in the analysis of Effective Component of Chinese Medicine.
(5) supercritical fluid chromatography analytic approach (SFC): SFC does with supercritical fluid a kind of chromatographic technique that mobile phase carries out analyzing, its supplementing as GC and HPLC, not only have the analyst coverage wider than GC and HPLC, and the detecting device that all GC and HPLC commonly use all can be used as SFC detecting device.
(6) mass spectrometric hyphenated technique analytic approach: mass spectrum (MS) is the most strong analysis tool analyzing pure organic compound, and mass spectrum can also provide molecular weight and structural information while detecting peak, makes detection have bidimensionality.Liquid-mass chromatography (LC-MS) and capillary electrophoresis-laser-induced fluorescence (CE-MS) development rapidly, have become the conventional method that Effective Component of Chinese Medicine is analyzed.
(7) infrared spectrum (IR) and Raman spectrum (Raman) analytic approach: utilize fourier transform raman spectroscopy technology (FT-Raman) and diffuse reflection FFIR technology (DF-FTIR) directly can differentiate raw medicinal herbs rapidly, utilizes diffuse reflection Fourier transform near infrared spectrometry can the component concentration of nondestruction quantitative analysis Chinese crude drug.
In sum, in Chinese Pharmacopoeia version in 2010, in Chinese crude drug, the detection of functional component mostly is high performance liquid chromatography, if but Chinese crude drug decocts means difference, whether the functional component in its dissolved element is identical with tradition, also needs to adopt high performance liquid chromatography to carry out studying and exploring further.
3, the analytical approach research of volatile compound in Chinese crude drug
(1) gas chromatography mass spectrometry method (GC-MS)
To the analysis of volatile matter in sample, gas chromatography-mass spectrography (GC-MS) is the method commonly used the most, sample mix odoring substance is separated by the centrifugation utilizing gas chromatography powerful, mass spectrum is utilized to be broken into pieces by the odoring substance of separation, form collection of illustrative plates, carry out library searching, qualification unknown material.
(2) gas chromatography-smell news (GC-O) method
Gas chromatography-smell news (GC-O) technology is rising in recent years, and it is effective especially to the research of food aroma.Some gas chromatographies-smell news technology the qualification and importance ranking that are used to Odor-active compound in food (aroma-active or odor-active) such as to analyze as CHARM (Combined hedonic aroma response measurement) analysis, aroma extract dilution analysis (aroma extract dilution analysis, AEDA), OSME analyze and detect frequency (detectionfrequency).GC-O technology has become a kind of method be widely used now, and the efficient separating power of gas chromatography and the sense of smell of human nose sensitivity combine by it.GC-O is called as " the state of the art ", i.e. current the most top, state-of-the-art technology.
But also there is not at present document to disclose employing gas chromatography-smell newss-mass spectroscopy to detect the feature imparting Odor-active compound in Chinese crude drug dissolved element.
Therefore, in prior art, effect material in Chinese crude drug and the feature in volatile matter are given to the research of the dissolving-out method of Odor-active material, it is generally the mode adopting traditional water decoction to boil, it is longer to there is the time of boiling medicine in the method, cannot extract the problem such as functional component and smell reactive compound comparatively up hill and dale at short notice.In addition, need to carry out pre-treatment before high performance liquid chromatography and gas chromatography on dissolved element-smell news-Mass Spectrometer Method, pre-treatment is generally comparatively loaded down with trivial details, in operation, may cause damage to the target component in decoction liquor, causes final measurement result to occur deviation; And do not have at present document openly to adopt gas chromatography-smell newss-mass spectroscopy to detect the feature imparting Odor-active compound in Chinese crude drug dissolved element yet.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of rapidly and efficiently stripping of Chinese crude drug composition and the Analysis and Identification method of dissolved element, in the method, the rapidly and efficiently stripping of Chinese crude drug composition adopts low pressure decocting method, low pressure decocting method decocting time is short, decoction efficiency is high, adopt effect material in high performance liquid chromatography qualitative and quantitative detection dissolved element and adopt gas chromatography-feature of smelling in news-mass spectroscopy qualitative and quantitative detection Chinese crude drug dissolved element to give Odor-active compound, efficiency is high.
Above-mentioned technical matters of the present invention can be achieved through the following technical solutions: a kind of rapidly and efficiently stripping of Chinese crude drug composition and the Analysis and Identification method of dissolved element, comprise the following steps:
(1) choose Chinese crude drug, adopt low pressure to decoct, decoct after terminating, obtain Chinese crude drug decoction liquor;
(2) get the Chinese crude drug decoction liquor in step (1), adopt the high performance liquid chromatography of Chinese Pharmacopoeia version in 2010, qualitative and quantitative analysis is carried out to the functional component in Chinese crude drug decoction liquor;
(3) the Chinese crude drug decoction liquor in step (1) is got, adopt the volatile matter in Headspace-solid phase microextraction method extraction Chinese crude drug decoction liquor, employing gas chromatography-smelling the feature imparting Odor-active compound of news-mass spectroscopy to the volatile matter in Chinese crude drug decoction liquor carries out qualitative and quantitative analysis and qualification.
In the rapidly and efficiently stripping of above-mentioned Chinese crude drug composition and the authentication method of dissolved element:
The decoction pressure that low pressure described in step (1) decocts is preferably 0 ~ 101kPa but does not comprise 0kPa.With decoct pressure be about 55kPa time, decoct efficiency higher.
The temperature that low pressure described in step (1) decocts is preferably 50 ~ 120 DEG C, and the time is preferably 5s ~ 1h.When decoction temperature is 100 ~ 120 DEG C, decoct efficiency higher.
Described low pressure decocts the solvent adopted and is preferably water, described Chinese crude drug and water be preferably 1g:20 ~ 50mL with magnitude relation.
The particle diameter of the Chinese crude drug in step (1) is preferably 24 ~ 1000 orders.When Chinese crude drug particle diameter is 24 ~ 1000 order, granules swell, fully without caking, is suitable for test.
Decoct in step of the present invention (1) and adopt environment under low pressure decocting herb, improve decoction efficiency on the one hand, shorten the time of boiling medicine, achieve the object extracting functional component and smell reactive compound within a short period of time; On the other hand, before upper machine, the pretreatment process of sample is simple, traditional pretreatment process, need complicated technologies such as extracting, concentrated, and in the present invention when the analysis of high performance liquid chromatography centering decocted liquid medicine functional component, direct injected after film crossed by most decoction liquor sample, farthest can not only reduce the loss of target component, can also save the pre-treatment time of traditional analysis.
The high performance liquid chromatography of Chinese Pharmacopoeia version in 2010 is adopted in step (2), when qualitative and quantitative analysis is carried out to the functional component in Chinese crude drug decoction liquor, the parameter arranging high performance liquid chromatography is preferably: the online degas system of HPLC system disposition G1322A vacuum, G1311A four-stage pump, G1329A automatic sampler, G1316A column oven and G1315D DAD detecting device, chromatographic column is Agilent SB-C18 chromatographic column.
Retention time comparison and n-compound is adopted to verify that these two kinds of qualification modes carry out qualitative and quantitative analysis to the functional component in Chinese crude drug in step (2).
During the volatile matter adopting Headspace-solid phase microextraction method to extract in Chinese crude drug decoction liquor in step (3), the extracting head of Solid-phase Microextraction preferably adopts PDMS/DVB/CAR tri-coating extracting head.
During the volatile matter adopting Headspace-solid phase microextraction method to extract in Chinese crude drug decoction liquor in step of the present invention (3), one of preferred embodiment can be: the decocting for Chinese herbal medicine liquid getting 20mL, under 60 DEG C of conditions, balance 20min, adopt PDMS/DVB/CAR tri-coating extracting head absorption 40min.
Compare traditional solvent extraction, adopt Headspace-solid phase microextraction method have simple to operate, without advantages such as artifact formation, effect of extracting are better; And without the need to a large amount of solvent, extraction time is short, extraction efficiency is high.
When adopting in step (3) gas chromatography-the smell feature imparting Odor-active compound of newss-mass spectroscopy to the volatile matter in Chinese crude drug decoction liquor to carry out qualitative and quantitative analysis, the parameter of gas chromatography is preferably: chromatography capillary tubing string is DB-WAX, initial temperature is preferably 40 DEG C, keep 3min, then preferably 200 DEG C are warmed up to the programming rate of 5 DEG C/min, be preferably again and be warmed up to 230 DEG C of maintenance 3min with the programming rate of 10 DEG C/min, carrier gas is helium, constant flow rate is preferably 1.2mL/min, injector temperature is preferably 250 DEG C, pressure is preferably 14.87psi, split ratio is preferably 1:1, mass spectrometry parameters is: electron impact ion source, and electron energy is preferably 70eV, and transmission line temperature is preferably 280 DEG C, ion source temperature is preferably 230 DEG C, quadrupole rod temperature is preferably 150 DEG C, and solvent delay is preferably 3min, and mass scan range m/z is preferably 55 ~ 500, the parameter of olfactometry device is: interface temperature is preferably 200 DEG C.
These four kinds of qualification modes are given Odor-active compound to the feature in Chinese crude drug and are carried out analysis and identification to adopt linear retention index comparison, odor property, NIST library searching and n-compound to verify in step (3).
Compared with prior art, tool of the present invention has the following advantages:
(1) adopt environment under low pressure decocting herb in the present invention, improve decoction efficiency, shorten the time of boiling medicine, achieve the object extracting functional component and smell reactive compound within a short period of time;
(2) the present invention adopts environment under low pressure decocting herb, on dissolved element, before machine, pre-treatment is simple, farthest can reduce the loss of target component, the analysis of high performance liquid chromatography centering decocted liquid medicine functional component, major part can adopt decoction liquor to cross the method for direct injected after film, this, compared with general pretreatment process (as extracted, concentrating), farthest can not only reduce the loss of target component, and save the pre-treatment time of traditional analysis;
(3) the present invention is directed to the volatile matter in Chinese crude drug decoction liquor, adopt Headspace-solid phase microextraction method have simple to operate, without advantages such as artifact formation, effect of extracting are better; And without the need to a large amount of solvent, extraction time is short, extraction efficiency is high;
(4) the present invention carries out rapidly and efficiently stripping by utilizing low pressure decocting method to traditional Chinese medicine ingredients, the functional component in high performance liquid chromatography centering decocted liquid medicine is adopted to analyze, adopt gas chromatography-feature of smelling in news-mass spectroscopy (GC-O-MS) centering decocted liquid medicine to give Odor-active compound and carry out qualitative and quantitative analysis, for the instant edible of Chinese medicine and herbal cuisine opens new method.
Accompanying drawing explanation
Fig. 1 is traditional decoction method American Ginseng decoction liquor GC-O-MS total ion current figure in embodiment 1;
Fig. 2 adopts low pressure decocting method American Ginseng decoction liquor GC-O-MS total ion current figure of the present invention in embodiment 1;
Fig. 3 is the HPLC-DAD chromatogram of American Ginseng decoction liquor in embodiment 1;
Fig. 4 is traditional decoction method Radix Angelicae Sinensis decoction liquor GC-O-MS total ion current figure in embodiment 2;
Fig. 5 adopts low pressure decocting method Radix Angelicae Sinensis decoction liquor GC-O-MS total ion current figure of the present invention in embodiment 2;
Fig. 6 is the HPLC-DAD chromatogram of Radix Angelicae Sinensis decoction liquor in embodiment 2;
Fig. 7 is traditional decoction method chrysanthemum decoction liquor GC-O-MS total ion current figure in embodiment 3;
Fig. 8 adopts low pressure decocting method chrysanthemum decoction liquor GC-O-MS total ion current figure of the present invention in embodiment 3;
Fig. 9 is the HPLC-DAD chromatogram of chrysanthemum decoction liquor in embodiment 3;
Figure 10 is traditional decoction method Radix Astragali decoction liquor GC-O-MS total ion current figure in embodiment 4;
Figure 11 adopts low pressure decocting method Radix Astragali decoction liquor GC-O-MS total ion current figure of the present invention in embodiment 4;
Figure 12 is the HPLC-DAD chromatogram of Radix Astragali decoction liquor in embodiment 4;
Figure 13 is traditional decoction method honeysuckle decoction liquor GC-O-MS total ion current figure in embodiment 5;
Figure 14 adopts low pressure decocting method honeysuckle decoction liquor GC-O-MS total ion current figure of the present invention in embodiment 5;
Figure 15 is the HPLC-DAD chromatogram of honeysuckle decoction liquor in embodiment 5;
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Embodiment
The rapidly and efficiently stripping of embodiment 1 American Ginseng composition and authentication method
To ginsenoside Rg in American Ginseng
1, ginsenoside Re, ginsenoside Rb
1the content of these 3 kinds of main pharmacodynamics compositions carries out high-performance liquid chromatogram determination.In all volatile constituents of American Ginseng, what content was the highest is (Z)-9-17 alkene-4,6-diine-8-alcohol, and it is unsaturated alcohol compounds, and alcohols and the compound containing unsaturated link have anti-oxidant and effect that is scavenging free radicals.Secondly higher composition is phytosterin compound, and in American Ginseng, content is 19.05%, has and reduces serum cholesterol, anticancer and anti-aging effects.Adopt volatile ingredient in Solid-phase Microextraction extraction American Ginseng decoction liquor, use high-efficient liquid phase chromatogram technique analysis functional component wherein, re-use gas chromatography-smell news-mass-spectrometric technique qualitative and quantitative analysis and go out crucial Odor-active compound wherein.
1, material
(1) sample American Ginseng
(2) reagent and instrument
Standard reference compounds equal purchased from American Sigma company, chromatographically pure.
The analysis of functional component in Chinese crude drug, adopts the high performance liquid chromatography in Chinese Pharmacopoeia version in 2010.
The analytical instrument of Chinese crude drug functional component is: the online degas system of HPLC system disposition G1322A vacuum, G1311A four-stage pump, G1329A automatic sampler, G1316A column oven and G1315D DAD detecting device.
Gas chromatography-smell news-mass spectrometer: compounds GC-MS INSTRUMENT MODEL, 7890A-7000B (triple level Four bar mass spectrometer-QQQ), purchased from American Agilent company; Smell taste detector: Sniffer 9000, purchased from Brechb ü hler company of Switzerland; Chromatographic column: DB-Wax (30m × 0.25mm × 0.25 μm), purchased from American J & W company; Hand sampling handle purchased from American Supelco company; SPME extracts syringe needle (DVB/CAR on PDMS) purchased from American Supelco company; Ml headspace bottle (40mL) purchased from American QEC company.
2, analysis condition
(1) analysis condition of functional component in decocting for Chinese herbal medicine liquid
The online degas system of HPLC system disposition G1322A vacuum, G1311A four-stage pump, G1329A automatic sampler, G1316A column oven and G1315D DAD detecting device, chromatographic column is Agilent SB-C
18(5 μm, 4.6 × 250mm) chromatographic column, it is 30 DEG C that column temperature controls, and mobile phase is the phosphoric acid solution of acetonitrile and 0.1% massfraction, and flow velocity is 1mL/min, DAD determined wavelength is 203nm, adopts acetonitrile-aqueous solution gradient elution, as table 1.
Table 1 gradient elution program
(2) in decocting for Chinese herbal medicine liquid, the GC-O-MS analysis condition of Odor-active compound is:
Gas chromatography (GC) condition: chromatography capillary tubing string is DB-WAX (30m × 0.25mm × 0.25 μm), initial temperature 40 DEG C, keep 3min, then be warmed up to 200 DEG C with the programming rate of 5 DEG C/min, then be warmed up to 230 DEG C of maintenance 3min with the programming rate of 10 DEG C/min, carrier gas is helium (He), constant flow rate is 1.2mL/min, injector temperature 250 DEG C, pressure 14.87psi, split ratio 5:1.
Mass Spectrometry Conditions (MS): electronics bombardment (electron impact, EI) ion gun, electron energy 70eV, transmission line temperature 280 DEG C, ion source temperature is 230 DEG C, and quadrupole rod temperature is 150 DEG C, solvent delay 3min, mass scan range m/z 55 ~ 500.
Olfactometry device: interface temperature is 200 DEG C.Smell news result error to prevent valuation officer's mycteroxerosis from causing during detection, and need to pass into moistening air.
(3) enrichment of volatile ingredient in decocting for Chinese herbal medicine liquid
Solid phase micro-extraction technique (SPME): solid-phase micro-extracting device extracts syringe needle by SPME handle, SPME and ml headspace bottle is formed, in sample pretreatment process, 10mL decocting for Chinese herbal medicine liquid is added respectively in 40mL ml headspace bottle, and at 60 DEG C of Water Under bath balance 20min.After water-bath balance, insert solid-phase microextraction syringe needle, the extracting head of Solid-phase Microextraction adopts PDMS/DVB/CAR tri-coating extracting head, headspace absorption 40min.After absorption, extraction pin is inserted in gas chromatograph injection port and resolve 3min under 250 DEG C of conditions, analyzed by GC-MS, obtain the total ion current figure of aroma compound.
3, analytical approach
(1) GC-O-MS analyzes
I. qualitative analysis
Linear retention index (LRI value), odor property (odor property) comparison, NIST2.0 library searching and n-compound checking qualification mode is adopted jointly to complete to the qualification of unknown compound.Wherein: NIST2.0 library searching is composed in storehouse at NIST by the smell unknown compound in mass spectrogram to retrieve, and requires positive and negative matching degree>=800 of compound retrieved; Linear retention index (LRI value), odor property (odor property) Comparison Method are with C
6~ C
25n-alkane adopt the heating schedule identical with testing sample as standard, calculate the RI value of unknown compound, and compare in conjunction with odor characteristics and the RI that drafts compound, thus method is qualitatively carried out to material; N-compound checking is by the compound of Preliminary Identification, analyze according to the heating schedule sample introduction that sample GC-O-MS is identical with its corresponding standard items, finally compare both RI values, odor characteristics and library searching matching degree, thus determine whether this compound.
II. quantitative test
The quantitative test of centering decocted liquid medicine Odor-active compound mainly adopts internal standard method.2-methyl-3 heptanone that concentration is 0.816 μ g/ μ L is added in 10mL (or 15mL) decoction liquor to be analyzed.By the proportionate relationship of internal standard compound peak area and concentration and Odor-active compound to be measured, calculate the content of respective substance.This quantivative approach fast, efficiently.
(2) HPLC-DAD analyzes
I. qualitative analysis
In centering decocted liquid medicine, the qualitative analysis of targeted efficacy composition mainly adopts n-compound authentication method.Under identical chromatographic condition, the targeted efficacy material retention time in the standard items of targeted efficacy material and decoction liquor is compared, qualitatively determine corresponding effect material.
II. quantitative test
In centering decocted liquid medicine, the quantitative test of targeted efficacy composition mainly adopts external standard method, by drawing standard curve, and accurate quantitative analysis.
4, measurement result
(1) Odor-active compound in American Ginseng decoction liquor
I. traditional decoction method
Traditional decoction method is with heating by electric cooker, and amount of water is 30mL, and carry out decocting for 2 hours to 1g American Ginseng powder, its total ion current figure is as Fig. 1, and Odor-active compound is as following table.
Odor-active compound in table 2 traditional decoction method American Ginseng decoction liquor
II. low-pressure machine decocting method
Low-pressure machine decocting method adopts low-pressure machine, and decocting pressure is about 55kPa, and amount of samples, the water yield and temperature are with traditional decocting method, and decocting time is 3min, and under the method, total ion current figure is as Fig. 2, and in decoction liquor, Odor-active compound is as table 3.
Odor-active compound in table 3 low pressure decocting method American Ginseng decoction liquor
In these two kinds of method gained decoction liquor, compare from overall look and feel, difference is little.By analysis result, we find, in two kinds of decoction liquor the kind of main flavor and content basically identical, and the kind of low pressure decocting method gained flavor substance is more.
(2) effect material in American Ginseng decoction liquor
I. the contrast of two kinds of decocting methods
Detect 3 kinds of functional component content in American Ginseng decoction liquor with HPLC-DAD, its chromatogram is as Fig. 3, and retention time corresponding to ginsenoside Rg1, ginsenoside Re and ginsenoside Rb1 is respectively 34.611,35.238 and 52.936.Shown in Fig. 3,3 kinds of effect separating substances effects are better.Compare the content of 3 kinds of functional components in traditional decoction method and low pressure decocting method gained American Ginseng decoction liquor, result is as table 4.
The contrast (μ g/ μ L) of the different decocting method effect content of material of two kinds, table 4
Discovery is compared by data, traditional decoction method is better to the result of extraction of 3 kinds of effect materials in American Ginseng, for American Ginseng, long decoction advantageously, decoct the stripping quantity that efficiency is general objective effect material in the unit interval, it is 26.1390/120=0.2178 (μ g/ μ L*min) that traditional decoction method 2 hours (120min) decocts efficiency, and it is 16.2556/3=5.4185 (μ g/ μ L*min) that low-pressure machine decoction 180s (3min) decocts efficiency.Therefore, although low-pressure machine decoction gained effect total amount is high not as traditional decoction, comparatively traditional decoction is high 24.88 times for the decoction efficiency of low-pressure machine!
II. the optimization of low-pressure machine decocting condition
A. low-pressure machine setting parameter
A. humid test
Temperature range 50 DEG C ~ 120 DEG C, studies 50 DEG C, 70 DEG C, 85 DEG C, 100 DEG C and 120 DEG C respectively.
B. digestion time test
Decocting time scope: 5s ~ 1h, studies 5s, 900s, 1800s, 2700s and 3600s (1h) respectively.
B. the selection of Chinese medicine granularity
A certain amount of herb powder is filled, about this powder volume accounts for the half of whole container volume in container.Through repeatedly verifying, should choose after consumption and granularity decoct in low-pressure machine, particle fully swelling (taking the volume of whole capsule) is without caking, empirical tests finds, when the granularity of Chinese medicinal granule is 24 ~ 1000 order, granules swell, fully without caking, is suitable for test.
C. the measurement result under low-pressure machine different parameters condition
Table 5 low-pressure machine different parameters condition decocts American Ginseng effect content of material (unit: μ g/ μ L)
As can be seen from Table 5, when decoction pressure is about 55kPa, temperature is 50 ~ 120 DEG C, when vacuum time is 5 ~ 3600s, ginsenoside Rg1, ginsenoside Re and ginseng soap Rb1 content are higher, when temperature is about 100 DEG C, ginsenoside Rg1, ginsenoside Re and ginseng soap Rb1 content are higher.
The rapidly and efficiently stripping of embodiment 2 Radix Angelicae Sinensis composition and authentication method
Radix Angelicae Sinensis (Angelica sinensis) call dryly to return, the Qin which, western Radix Angelicae Sinensis, Min Radix Angelicae Sinensis, Radix Angelicae Sinensis, Radix Angelicae Sinensis body, contain and return tail, araliae cordatae per nnial herb, at distribution in China in Gansu, Yunnan, Sichuan, Qinghai, Shaanxi, Hunan, Hubei, the ground such as Guizhou, all there is cultivation various places.The root of Radix Angelicae Sinensis can be used as medicine, and is one of the most frequently used Chinese medicine.Radix Angelicae Sinensis also can be used in spiced and stewed food batching, and its principal feature is flavor and enhancing flavor, increases meat products and medicine fragrance.Medical value: enrich blood; Invigorate blood circulation; Menstruction regulating and pain relieving; Moisturize laxation; Its main composition is forulic acid and Ligustilide.
1, material
(1) sample Radix Angelicae Sinensis
(2) reagent and instrument are with embodiment 1.
2, analysis condition
(1) analysis condition of herbal function composition
Chromatographic column is Agilent SB-C18 (5 μm, 4.6 × 250mm) chromatographic column, and it is 25 DEG C that column temperature controls, and mobile phase is acetonitrile and 0.085% phosphoric acid solution, and flow velocity is 1mL/min, DAD determined wavelength is 325nm, adopts gradient elution, as table 6.
Table 6 gradient elution program
(2) in decocting for Chinese herbal medicine liquid, the GC-O-MS analysis condition of Odor-active compound is:
Gas chromatography (GC) condition, mass spectrum (MS) condition, olfactometry device are with embodiment 1.
(3) enrichment of volatile ingredient in decocting for Chinese herbal medicine liquid
Solid phase micro-extraction technique (SPME): with embodiment 1.
3, analytical approach
With American Ginseng decoction liquor analytical approach in embodiment 1.
4, measurement result
(1) Odor-active compound in Radix Angelicae Sinensis decoction liquor
I. traditional decoction method
Traditional decoction method is with heating by electric cooker, and amount of water is 100mL, and carry out decocting for 2 hours to 5g Chinese Angelica Root, its total ion current figure is as Fig. 4, and Odor-active compound is as table 7.
Table 7 traditional decoction method decocts Radix Angelicae Sinensis gained decoction liquor Odor-active compound
II. low pressure decocting method
Low pressure decocting method adopts low-pressure machine, and low-pressure machine decocting method adopts low-pressure machine, and decocting pressure is about 55kPa, amount of samples, the water yield and temperature are with traditional decocting method, and decocting time is 3min, under the method, total ion current figure is as Fig. 5, and in decoction liquor, Odor-active compound is as table 8.
Table 8 low-pressure machine decocting method decocts Odor-active compound in Radix Angelicae Sinensis gained decoction liquor
From table 8, we can find, the kind of two kinds of decocting method gained decoction liquor flavor substances is incomplete same.In Radix Angelicae Sinensis decoction liquor, the material of cyclenes hydro carbons is more, and they embody medicinal herbs breath.In overall look and feel, the difference of 2 kinds of method gained decoction liquor is little.
(2) effect material in Radix Angelicae Sinensis decoction liquor
I. the contrast of two kinds of decocting methods
Effect material main in Radix Angelicae Sinensis decoction liquor is forulic acid and Ligustilide.Detect these the 2 kinds of effect materials in decoction liquor with HPLC-DAD, its chromatogram is as Fig. 6.From diagram, two kinds of targeted efficacy separating substances effects are better.Wherein the retention time of forulic acid is 16.188, and the retention time of Ligustilide is 42.959.With these two kinds of compounds for targeted efficacy material, the decoction effect of comparative analysis 2 kinds of decocting methods, result is as table 9.
Table 9 two kinds of decocting methods decoct functional component content in Radix Angelicae Sinensis gained decoction liquor
Found by contrast, in 2 kinds of decocting method gained decoction liquor, 2 kinds of functional component comparision contents are close, and in low pressure decocting method, Ligustilide content is higher.This may be that in decoction liquor, content is lost because Ligustilide is being easier to volatilization for a long time.Decoct efficiency and refer to decoction gained general objective effect content of material between unit.The decoction efficiency of low-pressure machine 180s (3min) is 0.0251/3=0.0084 (μ g/ μ L*min), and the decoction efficiency of traditional decoction 2 hours (120min) is 0.0366/120=0.0084 (μ g/ μ L*min).It can thus be appreciated that omit many although traditional decoction method decocts Radix Angelicae Sinensis gained targeted efficacy content of material, the decoction efficiency of low-pressure machine is higher than classic method 28 times!
II. the optimization of low-pressure machine decocting condition
A. low-pressure machine setting parameter is with embodiment 1.
A. humid test is tested with embodiment 1 with embodiment 1, b. digestion time.
B. the selection of Chinese medicine granularity is with embodiment 1.
C. the measurement result under low-pressure machine different parameters condition
Table 10 low-pressure machine different parameters condition decocts Radix Angelicae Sinensis gained targeted efficacy content (unit: μ g/ μ L)
As can be seen from Table 10, when decoction pressure is about 55kPa, temperature is 50 ~ 120 DEG C, and when vacuum time is 5 ~ 3600s, forulic acid, Ligustilide content are higher.When temperature is 120 DEG C, forulic acid, Ligustilide are higher.
The rapidly and efficiently stripping of embodiment 3 chrysanthemum composition and authentication method
Chrysanthemum is the dry capitulum of feverfew chrysanthemum (Chrysanthemum mifolium Ramat), is China's conventional Chinese medicine, has effect of dispelling wind, heat-clearing, improving eyesight, removing toxic substances.The disease such as primary treatment headache, dizzy, hot eyes, ambition dysphoria with smothery sensation, furunculosis, pyogenic infections.Modern pharmacological research shows, chrysanthemum has treatment coronary heart disease, reduces blood pressure, prevents high fat of blood, antibacterial, antiviral, anti-inflammatory, anti-ageing multiple physiologically active of waiting for a long time.Current China Chrysanthemum morifolium commercially has 8 large main flow merchandise resourceses, is respectively Hang Ju, Bo chrysanthemum, tribute chrysanthemum, Chu chrysanthemum, Qi Ju, bosom chrysanthemum, Ji chrysanthemum, Huang Ju.Its main composition is chlorogenic acid, galuteolin and 3,5-Dicaffeoylquinic acid.
1, material
(1) sample chrysanthemum
(2) reagent and instrument are with embodiment 1.
2, analysis condition
(1) analysis condition of herbal function composition
Chromatographic column is Agilent SB-C18 chromatographic column (5 μm, 4.6 × 250mm) chromatographic column, and it is 30 DEG C that column temperature controls, and mobile phase is acetonitrile and 0.1% phosphoric acid solution, and flow velocity is 1mL/min, DAD determined wavelength is 348nm, adopts gradient elution, as table 11.
Table 11 gradient elution program
(2) in decocting for Chinese herbal medicine liquid, the GC-O-MS analysis condition of Odor-active compound is:
Gas chromatography (GC) condition, mass spectrum (MS) condition, olfactometry device are with embodiment 1.
(3) enrichment of volatile ingredient in decocting for Chinese herbal medicine liquid
Solid phase micro-extraction technique (SPME) is with embodiment 1.
3, analytical approach
With embodiment 1.
4, measurement result
(1) Odor-active compound in chrysanthemum decoction liquor
I. traditional decoction method
Traditional decoction method is with heating by electric cooker, and amount of water is 100mL, and carry out decocting for 2 hours to 2g chrysanthemum powder, its total ion current figure is as Fig. 7, and Odor-active compound is as 12.
Odor-active compound in table 12 traditional decoction method chrysanthemum decoction liquor
II. low pressure decocting method
Low-pressure machine decocting method adopts low-pressure machine, and decocting pressure is about 55kPa, and amount of samples, the water yield and temperature are with traditional decocting method, and decocting time is 3min, and under the method, GC-O-MS total ion current figure is as Fig. 8, and in decoction liquor, Odor-active compound is as table 13.
Odor-active compound in table 13 low pressure decocting method chrysanthemum decoction liquor
Find by comparing two kinds of different decocting method gained Odor-active compounds, in decoction liquor, Odor-active compound is basically identical, and low-pressure machine decocting method gained classes of compounds is less, and from overall sense organ, both difference is little.
(2) effect material in chrysanthemum decoction liquor
I. the contrast of two kinds of decocting methods
Effect material main in chrysanthemum decoction liquor is chlorogenic acid, galuteolin and 3,5-Dicaffeoylquinic acid.Measure these 3 kinds of functional components in decoction liquor with HPLC-DAD, gained chromatogram is as Fig. 9.From chromatogram 9,3 kinds of targeted efficacy separating substances effects are better.The retention time of chlorogenic acid, galuteolin and 3,5-Dicaffeoylquinic acid is respectively 9.258min, 20.023min and 26.686min.With these three kinds of compounds for targeted efficacy material, the decoction effect of comparative analysis two kinds of decocting methods, result is as following table 14.
Table 14 two kinds of decocting methods decoct functional component content (μ g/ μ L) in chrysanthemum gained decoction liquor
Found by contrast, in 2 kinds of decocting method gained decoction liquor, except galuteolin, functional component comparision contents is close.Decoct efficiency by calculating, comparatively classic method is high 26.5 times for the decoction efficiency of low-pressure machine!
II. the optimization of low-pressure machine decocting condition
A. low-pressure machine setting parameter is with embodiment 1.
A. humid test is tested with embodiment 1 with embodiment 1, b. digestion time.
B. the selection of Chinese medicine granularity is with embodiment 1.
C. the measurement result under low-pressure machine different parameters condition
Table 15 low-pressure machine different parameters condition decocts chrysanthemum gained targeted efficacy content (unit: μ g/ μ L)
As can be seen from Table 15, when decoction pressure is about 55kPa, temperature is 50 ~ 120 DEG C, and when vacuum time is 5 ~ 3600s, chlorogenic acid, galuteolin and 3,5-Dicaffeoylquinic acid equal size are higher; When temperature is 100 DEG C, chlorogenic acid, galuteolin and 3,5-Dicaffeoylquinic acid equal size are higher.
The rapidly and efficiently stripping of embodiment 4 astragalus root components and authentication method
The Radix Astragali, has another name called continuous stilbene.Perennial herb, high 50-100cm.Main root is plump, wooden, normal branch, canescence.Stem is upright, and top multi-branched, has thin rib, by white pubescence.Perennial herb, high 50-100cm.Originate in the ground such as the Inner Mongol, Shanxi, Gansu, Heilungkiang.The history of medicinal existing more than 2000 year so far of the Radix Astragali, it has enhanced machine body immunity function, protects the liver, diuresis, anti-ageing, resisting stress, step-down and antibacterial action more widely, its main composition is Calycosin-7-O-BETA-D-glucoside.
1, material
(1) the sample Radix Astragali
(2) reagent and instrument are with embodiment 1.
2, analysis condition
(1) analysis condition of herbal function composition
Chromatographic column is Agilent SB-C18 chromatographic column (5 μm, 4.6 × 250mm) chromatographic column, and it is 30 DEG C that column temperature controls, and mobile phase is acetonitrile and 0.2% formic acid solution, and flow velocity is 1mL/min, DAD determined wavelength is 260nm.Adopt gradient elution, as table 16.
Table 16 gradient elution program
(2) in decocting for Chinese herbal medicine liquid, the GC-O-MS analysis condition of Odor-active compound is:
Gas chromatography (GC) condition, mass spectrum (MS) condition, olfactometry device are with embodiment 1.
(3) enrichment of volatile ingredient in decocting for Chinese herbal medicine liquid
Solid phase micro-extraction technique (SPME) is with embodiment 1.
3, analytical approach
With embodiment 1.
4, measurement result
(1) Odor-active compound in Radix Astragali decoction liquor
I. traditional decoction method
Traditional decoction method is with heating by electric cooker, and amount of water is 100mL, carries out decocting for 2 hours to 2g Milkvetch Root.Total ion current figure is as Figure 10, and Odor-active compound is as table 17.
Odor-active compound in table 17 traditional decoction method Radix Astragali decoction liquor
II. low-pressure machine decocting method
Low-pressure machine decocting method adopts low-pressure machine, and decocting pressure is about 55kPa, and amount of samples, the water yield and temperature are with traditional decocting method, decocting time is 3min, under the method, decoction liquor GC-O-MS total ion current figure is as Figure 11, and in decoction liquor, Odor-active compound is as table 18.
Odor-active compound in table 18 low-pressure machine decocting method Radix Astragali decoction liquor
Find by comparing two kinds of different decocting method gained Odor-active compounds, in decoction liquor, Odor-active compound is basically identical.From overall sense organ, both difference is little.
(2) effect material in Radix Astragali decoction liquor
I. the contrast of two kinds of decocting methods
Effect material main in Radix Astragali decoction liquor is calycosin heteroside.Detect this effect material with HPLC-DAD, its chromatogram is as Figure 12, and Calycosin-7-O-BETA-D-glucoside retention time is 6.033, and the decoction effect of comparative analysis two kinds of decocting methods, result is as table 19.
Table 19 two kinds of decocting methods decoct functional component content in Radix Astragali gained decoction liquor
Found by contrast, in 2 kinds of decocting method gained decoction liquor, the Calycosin-7-O-BETA-D-glucoside content of traditional decoction method is higher, but by comparing decoction efficiency, it is high 19.77 times that low pressure decocting method decocts efficiency than traditional decoction method!
II. the optimization of low-pressure machine decocting condition
A. low-pressure machine setting parameter is with embodiment 1.
A. humid test is tested with embodiment 1 with embodiment 1, b. digestion time.
B. the selection of Chinese medicine granularity is with embodiment 1.
C. the measurement result under low-pressure machine different parameters condition
Table 20 different parameters condition decocts functional component content in Radix Astragali decoction liquor
As can be seen from Table 20, when decoction pressure is about 55kPa, temperature is 50 ~ 120 DEG C, and when vacuum time is 5 ~ 3600s, Calycosin-7-O-BETA-D-glucoside (ng/ μ L) extraction efficiency is higher.Especially when temperature is 100 ~ 120 DEG C, extractive content is higher, and when extraction time is 900s ~ 1800s, extractive content is higher.
The rapidly and efficiently stripping of embodiment 5 honeysuckle composition and authentication method
Honeysuckle, has another name called honeysuckle (Lonicera japonica)." honeysuckle " one comes from Compendium of Material Medica, owing to opening as white at the beginning of FLOSLONICERAE, after transfer yellow to, hence obtain one's name honeysuckle.Medicinal material honeysuckle is Caprifoliaceae woodbine honeysuckle and congener dry flower or is with the flower just opened.Honeysuckle is described as clearing heat and detoxicating good medicine from ancient times.Its property sweet cold air fragrance, clear heat with drugs of sweet flavour and cold nature and not injuring one's stomach, fragrance thoroughly reaches and can be eliminating evil.Honeysuckle can dispelling wind-heat, also kind removing summer-heat blood poison, for various febrile disease, as the disease such as body heat, dermexanthesis, spot, hot carbuncle carbuncle, abscess of throat, and equal Be very effective.The functional component of honeysuckle is chlorogenic acid and galuteolin.
1, material
(1) sample honeysuckle.
(2) reagent and instrument are with embodiment 1.
2, analysis condition
(1) analysis condition of herbal function composition
Chromatographic column is Agilent SB-C18 chromatographic column (5 μm, 4.6 × 250mm) chromatographic column, and it is 30 DEG C that column temperature controls, and mobile phase is acetonitrile and 0.5% acetic acid solution, and flow velocity is 1mL/min, DAD determined wavelength is 350nm, sample size 5 μ L.Adopt gradient elution, as table 21.
Table 21 gradient elution program
(2) in decocting for Chinese herbal medicine liquid, the GC-O-MS analysis condition of Odor-active compound is:
Gas chromatography (GC) condition, mass spectrum (MS) condition, olfactometry device are with embodiment 1.
(3) enrichment of volatile ingredient in decocting for Chinese herbal medicine liquid
Solid phase micro-extraction technique (SPME): with embodiment 1.
3, analytical approach
With embodiment 1.
4, measurement result
(1) Odor-active compound in honeysuckle decoction liquor
I. traditional decoction method
Traditional decoction method is with heating by electric cooker, and amount of water is 80mL, carries out decocting for 2 hours to 2g Honeysuckle Flower.Its decoction liquor GC-O-MS total ion current figure is as Figure 13.Odor-active compound is as table 22.
Odor-active compound in table 22 traditional decoction method honeysuckle decoction liquor
II. low pressure decocting method
Low-pressure machine decocting method adopts low-pressure machine, and decocting pressure is about 55kPa, and amount of samples, the water yield and temperature are with traditional decocting method, decocting time is 3min, under the method, its GC-O-MS total ion current figure is as Figure 14, and in decoction liquor, Odor-active compound is as table 23.
Odor-active compound in table 23 low-pressure machine decocting method honeysuckle decoction liquor
Find by comparing two kinds of different decocting method gained Odor-active compounds, the Odor-active classes of compounds in low-pressure machine decocting method gained decoction liquor is more, mainly presents the odor characteristics of the fragrance of a flower, medicine perfume (or spice).From overall sense organ, the odor characteristics difference of two kinds of decoctions is little.
(2) effect material in honeysuckle decoction liquor
I. the contrast of two kinds of decocting methods
Effect material main in honeysuckle decoction liquor is chlorogenic acid and galuteolin.This two kinds of targeted efficacy materials are detected with HPLC-DAD, its chromatogram is as Figure 15, and the retention time of chlorogenic acid is 8.182, and the retention time of galuteolin is 19.385, decoction effect when comparative analysis traditional decoction method decocts for 2 hours and low-pressure machine decocting time is 90s, result is as table 24.
Table 24 two kinds of decocting methods decoct functional component content in honeysuckle gained decoction liquor
Found by contrast, in 2 kinds of decocting method gained decoction liquor, effect content of traditional decoction method is higher, but decocts efficiency discovery by comparing, and low-pressure machine decocting method decocts efficiency, and comparatively traditional decoction method is high 35 times!
II. the optimization of low-pressure machine decocting condition
A. low-pressure machine setting parameter is with embodiment 1.
A. humid test is tested with embodiment 1 with embodiment 1, b. digestion time.
B. the selection of Chinese medicine granularity is with embodiment 1.
C. the measurement result under low-pressure machine different parameters condition
Table 25 different parameters condition decocts functional component content in honeysuckle decoction liquor
As can be seen from Table 25, when decoction pressure is about 55kPa, temperature is 50 ~ 120 DEG C, and when vacuum time is 5 ~ 3600s, the extractive content such as galuteolin and chlorogenic acid is higher, within the scope of 50 ~ 120 DEG C, extractive content difference is little, and when being about 100 DEG C with temperature, extractive content is relatively high, extraction time, extractive content was relatively high in 5s ~ 1800s.
Therefore, the present invention carries out rapidly and efficiently stripping by utilizing low pressure decocting method to traditional Chinese medicine ingredients, the functional component in high performance liquid chromatography centering decocted liquid medicine is adopted to analyze, adopt gas chromatography-feature of smelling in news-mass spectroscopy (GC-O-MS) centering decocted liquid medicine to give Odor-active compound and carry out qualitative and quantitative analysis, for the instant edible of Chinese medicine and herbal cuisine opens new method.
Although, above with general explanation, embodiment and test, the present invention is described in detail, but on basis of the present invention, can make some modifications or improvements it, the pressure that such as low pressure decocts, except the data near the 55kPa that adopts in above-described embodiment, can also be that other data within 0 ~ 100kPa described in claims of the present invention are as 10kPa, 15kPa, 20kPa, 25kPa, 30kPa, 40kPa, 60kPa, 70kPa, 80kPa, 90kPa, 100kPa etc., temperature parameter is as 50 DEG C, 60 DEG C, 80 DEG C, 70 DEG C, 90 DEG C, 110 DEG C, 120 DEG C, time parameter 5s, 10s, 20s, 100s, 1200s, 1800s, 2400s, 3600s etc., this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (9)
1. the rapidly and efficiently stripping of Chinese crude drug composition and an Analysis and Identification method for dissolved element, is characterized in that comprising the following steps:
(1) choose Chinese crude drug, adopt low pressure to decoct, decoct after terminating, obtain Chinese crude drug decoction liquor;
(2) get the Chinese crude drug decoction liquor in step (1), adopt the high performance liquid chromatography of Chinese Pharmacopoeia version in 2010, qualitative and quantitative analysis is carried out to the functional component in Chinese crude drug decoction liquor;
(3) the Chinese crude drug decoction liquor in step (1) is got, adopt the volatile matter in Headspace-solid phase microextraction method extraction Chinese crude drug decoction liquor, employing gas chromatography-smelling the feature imparting Odor-active compound of news-mass spectroscopy to the volatile matter in Chinese crude drug decoction liquor carries out qualitative and quantitative analysis and qualification.
2. the rapidly and efficiently stripping of Chinese crude drug composition according to claim 1 and the Analysis and Identification method of dissolved element, is characterized in that: the decoction pressure that the low pressure described in step (1) decocts is 0 ~ 101kPa but does not comprise 0kPa.
3. the rapidly and efficiently stripping of Chinese crude drug composition according to claim 1 and 2 and the Analysis and Identification method of dissolved element, is characterized in that: the temperature that the low pressure described in step (1) decocts is 50 ~ 120 DEG C, and the time is 5s ~ 1h.
4. the rapidly and efficiently stripping of Chinese crude drug composition according to claim 3 and the Analysis and Identification method of dissolved element, is characterized in that: it is water that described low pressure decocts the solvent adopted, described Chinese crude drug and water be 1g:20 ~ 50mL with magnitude relation.
5. the rapidly and efficiently stripping of Chinese crude drug composition according to claim 1 and the Analysis and Identification method of dissolved element, it is characterized in that: the high performance liquid chromatography adopting Chinese Pharmacopoeia version in 2010 in step (2), when qualitative and quantitative analysis is carried out to the functional component in Chinese crude drug decoction liquor, arranging high performance liquid chromatography parameter is: the online degas system of HPLC system disposition G1322A vacuum, G1311A four-stage pump, G1329A automatic sampler, G1316A column oven and G1315D DAD detecting device, chromatographic column is Agilent SB-C18 chromatographic column.
6. the rapidly and efficiently stripping of Chinese crude drug composition according to claim 1 and the Analysis and Identification method of dissolved element, is characterized in that: adopt retention time comparison and n-compound to verify that these two kinds of qualification modes carry out qualitative and quantitative analysis to the functional component in Chinese crude drug in step (2).
7. the rapidly and efficiently stripping of Chinese crude drug composition according to claim 1 and the Analysis and Identification method of dissolved element, it is characterized in that: during the volatile matter adopting Headspace-solid phase microextraction method to extract in Chinese crude drug decoction liquor in step (3), the extracting head of Solid-phase Microextraction adopts PDMS/DVB/CAR tri-coating extracting head.
8. the rapidly and efficiently stripping of Chinese crude drug composition according to claim 1 and the Analysis and Identification method of dissolved element, it is characterized in that: when adopting in step (3) gas chromatography-the smell feature imparting Odor-active compound of newss-mass spectroscopy to the volatile matter in Chinese crude drug decoction liquor to carry out qualitative and quantitative analysis, the parameter of gas chromatography is: chromatography capillary tubing string is DB-WAX, initial temperature 40 DEG C, keep 3min, then 200 DEG C are warmed up to the programming rate of 5 DEG C/min, be warmed up to 230 DEG C with the programming rate of 10 DEG C/min again and keep 3min, carrier gas is helium, constant flow rate is 1.2mL/min, injector temperature 250 DEG C, pressure is 14.87psi, split ratio is 1:1, mass spectrometry parameters is: electron impact ion source, electron energy 70eV, transmission line temperature 280 DEG C, and ion source temperature is 230 DEG C, and quadrupole rod temperature is 150 DEG C, solvent delay 3min, mass scan range m/z55 ~ 500, arranging olfactometry device parameter is: interface temperature is 200 DEG C.
9. the rapidly and efficiently stripping of Chinese crude drug composition according to claim 1 and the Analysis and Identification method of dissolved element, is characterized in that: these four kinds of qualification modes are given Odor-active compound to the feature in Chinese crude drug and carried out analysis and identification to adopt linear retention index comparison, odor property, NIST library searching and n-compound to verify in step (3).
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Application publication date: 20150218 |
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