CN107436331B - The method for flashing index ingredient in gas chromatography measurement Sishen wan - Google Patents
The method for flashing index ingredient in gas chromatography measurement Sishen wan Download PDFInfo
- Publication number
- CN107436331B CN107436331B CN201710536087.8A CN201710536087A CN107436331B CN 107436331 B CN107436331 B CN 107436331B CN 201710536087 A CN201710536087 A CN 201710536087A CN 107436331 B CN107436331 B CN 107436331B
- Authority
- CN
- China
- Prior art keywords
- sishen wan
- sample
- sishen
- rutaecarpine
- isopsoralen
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
-
- 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
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
- G01N2030/126—Preparation by evaporation evaporating sample
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The present invention provides a kind of methods that flash distillation gas chromatography measures psoralen in Sishen wan, Isopsoralen, Dehydrodiisoeugenol, schizandrin, rutaecarpin and Rutaecarpine simultaneously, comprising: flash distillation gas chromatography detection Sishen wan sample obtains the qualitative analysis, external standard method establishes standard working curve, obtains 3 step of quantitative analysis results of index ingredient in Sishen wan sample；One aspect of the present invention flashes gas-chromatography and uses solid sample direct injected, is not necessarily to complex extraction process, solvent-free use, therefore easy to operate, environmental protection；On the other hand quantitative detection is carried out to index ingredient in Sishen wan by flash distillation gas chromatography, can effectively saves experimental period, simplifies experimental procedure；Therefore, quality evaluating method of the invention has the characteristics that simple and environmentally-friendly, efficient, which has very profound significance to Sishen wan quality evaluation.
Description
(1) technical field
The present invention relates to a kind of methods of index ingredient in flash distillation gas chromatography measurement Sishen wan, and in particular to a kind of
Flash distillation gas chromatography simultaneously measure psoralen in Sishen wan, Isopsoralen, Dehydrodiisoeugenol, schizandrin,
The method of rutaecarpin and Rutaecarpine.
(2) background technique
Sishen wan is a kind of Chinese patent drug name, is astringent prescription, has the effect of warming kidney for dispelling cold, relieving diarrhea with astringents, not for kidney yang
Diarrhea caused by foot symptoms include borborygmus abdominal distension, it is half congealed just before dawn rush down, deficiency of food is not changed, endless diarrhea, face Huang limb cold.Sishen wan is by Pork and beans
Cool, psoralea corylifolia, Schisandra chinensis and evodia rutaecarpa four traditional Chinese medicine and jujube, raw rubber are made, wherein bone fat fonifying life-gate fire, and cold dispelling is evil, are monarch drug in a prescription；
Evodia rutaecarpa warming spleen and stomach for dispelling cold, the warm taste of nutmeg, relieving diarrhea with astringents is ministerial drug；Schisandra chinensis astringency inducing is for adjutant；Ginger
Warm stomach cold dispelling, jujube strengthen the spleen and stomach, and are all to make medicine.
The Pharmacopoeia of the People's Republic of China (2015 editions) provide, psoralen and isopsorapen contains in every gram of Sishen wan
Amount summation must not be less than 3mg.The content of psoralen and isopsorapen is the main component of Effects of Bu Gu rouge, and " pharmacopeia "
The index substance of middle evaluation psoralea corylifolia raw medicinal herbs.There was only the significant substance of psoralea corylifolia to the quality evaluation of Sishen wan in " pharmacopeia "
Content requirement, and to other three tastes Chinese medicines (nutmeg, Schisandra chinensis and evodia rutaecarpa) without quality evaluation." pharmacopeia " (2015
Version) it provides, volatile oil content must not be lower than 6% in nutmeg, and Dehydrodiisoeugenol content must not be lower than 0.1%；Schisandra chinensis
The content of middle schizandrin must not be lower than 0.4%；The sum of content of rutaecarpin and Rutaecarpine must not be lacked in evodia rutaecarpa
In 0.15%, the content of limonin must not be lower than 0.2%.Since limonin is a kind of bitter substance, there is anti-inflammation and sterilization
Effect, the main active of but not evodia rutaecarpa medicinal material, thus general Study it is more be research rutaecarpin and Wu
The content of the fruit of medicinal cornel time alkali.Therefore, in order to which the index ingredient to four taste Chinese medicines in Sishen wan is analyzed, it is necessary to develop one
Kind can measure wherein psoralen, Isopsoralen, Dehydrodiisoeugenol, schizandrin, rutaecarpin and Wu Zhu simultaneously
The method of cornel time alkali.
Existing literature to psoralen and isopsorapen in psoralea corylifolia and Fructus Schisandrae alcohol first detection method,
Common method has thin-layered chromatography, liquid chromatography, gas chromatography etc., in nutmeg Dehydrodiisoeugenol and
Rutaecarpin and Rutaecarpine in evodia rutaecarpa use thin-layered chromatography and liquid chromatography；But it needs means of supercritical extraction, surpass
The cumbersome pretreatment modes such as sound extraction.Measurement to these substances in Sishen wan sample, generallys use liquid chromatography, in addition to
It needs outside cumbersome extraction process, different Detection wavelengths is needed to the detection of different material, further increase detection workload.
Therefore, the present invention is directed to develop to be not required to pre-treatment and to measure psoralen in Sishen wan, Isopsoralen, dehydrogenation two simultaneously different
The method of eugenol, schizandrin, rutaecarpin and Rutaecarpine.
(3) summary of the invention
It is an object of the present invention to provide a kind of flash distillation gas chromatographies to measure psoralen in Sishen wan, different psoralea corylifolia simultaneously
The method of element, Dehydrodiisoeugenol, schizandrin, rutaecarpin and Rutaecarpine.
The present invention adopts the following technical scheme:
A kind of flash distillation gas chromatography measure simultaneously psoralen in Sishen wan, Isopsoralen, Dehydrodiisoeugenol,
The method of schizandrin, rutaecarpin and Rutaecarpine, the method are as follows:
(1) flash distillation gas chromatography detection Sishen wan sample obtains the qualitative analysis
Sishen wan sample is ground into powder and is fitted into cracker, cracker is placed at gas chromatograph injection port,
The sample introduction when cracker temperature reaches 300~350 DEG C, is detected with gas chromatograph, obtains gas chromatogram, passes through contrast standard
Substance retention time obtains psoralen, Isopsoralen, Dehydrodiisoeugenol, schizandrin, Wu in Sishen wan sample
The qualitative analysis of fruit of medicinal cornel alkali and Rutaecarpine；
The testing conditions of the gas chromatograph are as follows: chromatographic column is low-pole column, TRB-5 quartz capillary column (30m ×
0.25mmi.d. × 0.25 μm film thickness, 5% methyl polysiloxane, the U.S.), column temperature rise program is 50 DEG C of initial temperature, with 5~10
DEG C/min (preferably 10 DEG C/min) rate is raised to 200 DEG C, then is raised to 300 DEG C with 3~5 DEG C/min (preferably 5 DEG C/min) rate, so
Afterwards in 300 DEG C of 5~15min of holding (preferably 10min)；Injector temperature is 280~320 DEG C (preferably 300 DEG C), detector temperature
For 280~320 DEG C (preferably 300 DEG C), 30~50:1 of split ratio；Carrier gas is nitrogen or helium, flow velocity 1.0mL/min；
Cracker condition: 300~350 DEG C of furnace temperature of cracking；Cracker with 300~350 DEG C of gas chromatograph interface temperature；
(2) external standard method establishes standard working curve
The standard items of psoralen, Isopsoralen, schizandrin are dissolved in methylene chloride, are configured to hybrid standard product
Solution I；The standard items of Dehydrodiisoeugenol, rutaecarpin, Rutaecarpine are dissolved in methylene chloride, are configured to hybrid standard
Product solution II；Using gas chromatograph testing conditions identical with step (1) and cracker condition, to hybrid standard product solution I,
II carries out flash distillation gas chromatography detection, gas chromatogram is obtained, with the concentration of each standard items in hybrid standard product solution I, II
Peak area value for each standard items in abscissa, gas chromatogram is that ordinate draws standard working curve, and then obtains standard
Linear equation；
In the hybrid standard product solution I, psoralen, Isopsoralen, schizandrin standard items concentration respectively
Stand alone as 20~10000mg/L, preferably 50~10000mg/L；
In the hybrid standard product solution II, the concentration of Dehydrodiisoeugenol, rutaecarpin, Rutaecarpine standard items
Respectively stand alone as 20~2000mg/L, preferably 50~2000mg/L；
(3) quantitative analysis results of index ingredient in Sishen wan sample are obtained
By in the gas chromatogram of Sishen wan sample obtained by step (1), psoralen, Isopsoralen, two isobutyl of dehydrogenation
Fragrant phenol, schizandrin, rutaecarpin and Rutaecarpine peak area value substitute into normal linearity equation obtained by step (2) respectively
In, and then the content of each index ingredient in Sishen wan sample is calculated.
In the present invention, in order to ensure the uniformity and representativeness of sample, the partial size of powdered Sishen wan Chinese patent drug sample is excellent
It is selected as 80~120 mesh.If commercially available solid-state Sishen wan Chinese patent drug does not exist with powdery form, need that it is carried out to crush pre- place
Reason, such as grinds it, crosses 80~120 meshes, powdered samples are made.
Compared with prior art, beneficial effect of the present invention is mainly reflected in: the present invention flashes gas chromatography while surveying
Determine psoralen, Isopsoralen, Dehydrodiisoeugenol, schizandrin, rutaecarpin and evodia rutaecarpa in Sishen wan sample
Secondary alkali content, on the one hand flash gas-chromatography use solid sample direct injected, be not necessarily to complex extraction process, solvent-free use,
Therefore easy to operate, environmental protection；On the other hand quantitative detection is carried out to index ingredient in Sishen wan by flash distillation gas chromatography,
Experimental period can effectively be saved, simplify experimental procedure；Therefore, quality evaluating method of the invention has simple and environmentally-friendly, efficient
The characteristics of, which has very profound significance to Sishen wan quality evaluation.
(4) Detailed description of the invention
Fig. 1: the flash distillation gas chromatography-mass spectrum total ion current figure of Sishen wan sample (Sishen wan 1) and 6 standard items；
Flash distillation gas chromatogram of Fig. 2: 7 commercially available Sishen wan samples at 300 DEG C.
(5) specific embodiment
The present invention is described further combined with specific embodiments below, but protection scope of the present invention is not limited in
This.
Embodiment 1: psoralen, Isopsoralen, Dehydrodiisoeugenol, schizandrin, Wu in Sishen wan sample
The qualitative analysis of fruit of medicinal cornel alkali and Rutaecarpine
(1) instrument and reagent
The Gc/ms Analyser (GC-MS) of U.S. ThermoFinnigan Trace DSQ；The U.S.
ThermoFinniganTrace GC Ultra gas chromatograph is matched hydrogen flame detector (FID)；Japanese Frontier PY-
3030D double click type longitudinal type micro furnace cracker.
Local Sishen wan sample is bought from each pharmacy, 120 meshes are crossed after grinding, are dried to constant weight in 60 DEG C, it is spare.
(2) experimental method
It accurately weighs Sishen wan sample (Sishen wan 1) powder 0.5mg and is packed into specimen cup, after being fixed on sample feeding rod, be packed into peace
Cracker above GC injection port, sample is in room temperature at this time.After cracker temperature reaches suitable temperature, sample introduction is pressed
Button, specimen cup fall into the furnace heart, and volatile component transient evaporation brings GC injection port by carrier gas, carries out gas chromatographic analysis.
U.S.'s ThermoFinnigan Trace GC Ultra gas chromatograph (TRB-5 quartz capillary column, 30m ×
0.25mmi.d. × 0.25 μm, 5% methyl polysiloxane of film thickness, the U.S.), Japanese Frontier PY-3040D double click type longitudinal type
Micro furnace cracker.
Flash gas phase condition: UA-5 metal capillary column (30m × 0.25mmi.d. × 0.25 μm, 5% methyl polysilicon of film thickness
Oxygen alkane, Japan) temperature program: 50 DEG C of initial temperature, 200 DEG C are raised to 10 DEG C/min rate, then be raised to 300 DEG C with 5 DEG C/min rate,
Keep 10min；Injector temperature is 300 DEG C, and detector temperature is 300 DEG C, split ratio 30:1；Carrier gas nitrogen or helium, flow velocity
1.0mL/min.Cracker condition: cracking furnace temperature: 300 DEG C；Cracker with 300 DEG C of gas chromatograph interface temperature.
Mass Spectrometry Conditions are as follows: electron impact ion source, 250 DEG C of ion source temperature, 300 DEG C of transmission line temperature, ionizing energy
70eV, 40~550m/z of ion scan range.
(3) results and discussion
Psoralen, Isopsoralen, Dehydrodiisoeugenol, schizandrin, rutaecarpin and Rutaecarpine are
Psoralea corylifolia, nutmeg, Schisandra chinensis and the index substance of the quality evaluation of evodia rutaecarpa in Sishen wan, therefore first to this in Sishen wan
6 ingredients carry out qualitative analysis.Fig. 1 is the flash distillation gas chromatography-mass spectrum of Sishen wan sample (S1 Sishen wan 1) and 6 standard items
Total ion current figure.As can be known from Fig. 1, there are 6 peaks and psoralen, Isopsoralen, two isobutyl of dehydrogenation fragrant in Sishen wan sample
Phenol, schizandrin, rutaecarpin are consistent with 6 standard items chromatographic peak retention times of Rutaecarpine；And by mass spectrum to four
6 peaks are compared with standard quality spectrogram in refreshing ball, it is found that mass spectrogram is corresponding with standard items in 6 peaks in Sishen wan,
There is no extra fragment information, illustrates that 6 substances are psoralen, Isopsoralen, Dehydrodiisoeugenol, schisandrol
First, rutaecarpin and Rutaecarpine, and do not have to interfere with other substances.It the results are shown in Table 1.
Table 1: psoralen in Sishen wan, Isopsoralen, Dehydrodiisoeugenol, schizandrin, rutaecarpin and
The qualitative results of Rutaecarpine
Embodiment 2: the investigation of reproducibility
U.S. Thermo Trace GC ultra gas chromatograph (TRB-5 metal capillary column, 30m × 0.25mmi.d.
× 0.25 μm, 5% methyl polysiloxane of film thickness, the U.S.), Japanese Frontier PY-3030D double click type longitudinal type micro furnace cracking
Device.
Gas phase condition: temperature program: 50 DEG C of initial temperature, 200 DEG C are raised to 10 DEG C/min rate, then with 5 DEG C/min rate liter
To 300 DEG C, 10min is kept；Injector temperature is 300 DEG C, and detector temperature is 300 DEG C, split ratio 30:1；Carrier gas nitrogen or helium
Gas, flow velocity 1.0mL/min.
Cracker condition: cracking furnace temperature: 300 DEG C；Cracker with 300 DEG C of gas chromatograph interface temperature.
3 parts of 1 sample 0.5mg of Sishen wan in the same manner as in Example 1 are accurately weighed respectively and are packed into specimen cup, are fixed on sample introduction
After bar, it is packed into the cracker being mounted on above GC injection port, sample is in room temperature at this time.When cracker temperature reaches 300 DEG C,
Sample introduction button is pressed, specimen cup falls into the furnace heart, and volatile component transient evaporation brings GC injection port by carrier gas, carries out GC analysis.
The reproducibility (being indicated with relative standard deviation (RSD)) of the absolute peak area in computer chromatography peak.The results show that peak area
RSD≤5.46%, illustrating to flash 0.5mg, 120 mesh Sishen wan powder samples at 300 DEG C, to can guarantee that experimental result obtains good
Good reproducibility.
Embodiment 3: the flash distillation gas chromatography exploitation of 6 index substances in Sishen wan
The gas chromatograph Japan Frontier PY-3030D double click type longitudinal type of U.S. ThermoFinnigan Trace is micro-
Type furnace cracker.
Gas phase condition are as follows: chromatographic column is TRB-5 quartz capillary column (30m × 0.25mmi.d. × 0.25 μm, film thickness 5%
Methyl polysiloxane, the U.S.) column temperature rise program be 50 DEG C of initial temperature, be raised to 200 DEG C with 10 DEG C/min rate, then with 5 DEG C/min
Rate is raised to 300 DEG C, keeps 10min；Injector temperature is 300 DEG C, and detector temperature is 300 DEG C, split ratio 30:1；Carrier gas is
Nitrogen or helium, flow velocity 1.0mL/min.
Cracker condition: cracking furnace temperature: 300 DEG C；Cracker with 300 DEG C of gas chromatograph interface temperature.
Psoralen, Isopsoralen and schizandrin standard items are made into the dichloromethane solution of 20-10000mg/L
(mixed mark), the methylene chloride that Dehydrodiisoeugenol, rutaecarpin and Rutaecarpine standard items are made into 20-2000mg/L is molten
Liquid (mixed mark), draws 1 microlitre of solution and is injected at specimen cup, after being fixed on sample feeding rod after its solvent volatilizes, loading is mounted on GC
Cracker above injection port, sample is in room temperature at this time.When cracker temperature reaches 300 DEG C, sample introduction button, sample are pressed
Cup falls into the furnace heart, mixes mark solution transient evaporation, brings GC injection port by carrier gas and carry out a point analysis of variance.
The parameters such as the linear of this method, detection limit and quantitative limit are investigated, the results are shown in Table 2.It can see from table 2, Psoralen
Rouge element, Isopsoralen and schizandrin are in 20-10000mg/L, Dehydrodiisoeugenol, rutaecarpin and Rutaecarpine
Linear good within the scope of 20-2000mg/L, r is greater than 0.99.6 substance detection limits are between 0.48-3.33mg/L, quantitative limit
Between 1.59-10.00mg/L.And RSD is less than 4.75% under 100mg/L and 1000mg/L concentration, therefore, it is considered that this method is quasi-
True property is good, can be used to measure psoralen, Isopsoralen, Dehydrodiisoeugenol, schizandrin, rutaecarpin and
Rutaecarpine.
The linear of 2:6 standard items of table, detection limit and quantitative limit result
Embodiment 4: psoralen, Isopsoralen, Dehydrodiisoeugenol, schizandrin, Wu in commercially available Sishen wan
The assay of fruit of medicinal cornel alkali and Rutaecarpine
Flash distillation gas chromatographic analysis carried out to 7 commercially available Sishen wan samples, measurement wherein psoralen, Isopsoralen,
The content of Dehydrodiisoeugenol, schizandrin, rutaecarpin and Rutaecarpine.
Fig. 2 is the flash distillation gas chromatogram of 7 Sishen wan samples.Table 3 is the quantitative result of 6 substances.It is neutralized from Fig. 2
As can be seen that all containing psoralen, Isopsoralen, Dehydrodiisoeugenol, schizandrin, Wu in 7 samples in table 3
Fruit of medicinal cornel alkali and Rutaecarpine, it is believed that in 7 Sishen wans containing psoralea corylifolia, nutmeg, Schisandra chinensis and evodia rutaecarpa this four
Kind Chinese medicine.According to " pharmacopeia " (2015 editions) regulations, the sum of the content of psoralen and isopsorapen need to be greater than in Sishen wan
3mg/g.And table 3 the results show that the sum of the content of psoralen and isopsorapen meets in 7 commercially available Sishen wan samples
States Pharmacopoeia specifications, therefore, it is considered that Sishen wan is up-to-standard.And Dehydrodiisoeugenol, schizandrin, rutaecarpin and Wu Zhu
The ingredient of these four substances of cornel time alkali content difference in different Sishen wans.
Psoralen, Isopsoralen, Dehydrodiisoeugenol, schizandrin, rutaecarpin in 3:7 Sishen wan of table
With the assay result (mg/g) of Rutaecarpine
Embodiment 5: Sishen wan sample mark-on reclaims test
U.S.'s ThermoFinnigan Trace gas chromatograph；Japanese Frontier PY-3030D double click type longitudinal type is micro-
Type furnace cracker.
Gas phase condition are as follows:
Chromatographic column is TRB-5 quartz capillary column (30m × 0.25mmi.d. × 0.25 μm, 5% methyl polysilicon oxygen of film thickness
Alkane, the U.S.) column temperature rise program be 50 DEG C of initial temperature, be raised to 200 DEG C with 10 DEG C/min rate, then be raised to 300 with 5 DEG C/min rate
DEG C, keep 10min；Injector temperature is 300 DEG C, and detector temperature is 300 DEG C, split ratio 30:1；Carrier gas be nitrogen or helium,
Flow velocity 1.0mL/min.
Cracker condition: cracking furnace temperature: 300 DEG C；300 DEG C of vapor-phase thermal cracking device interface temperature.
Mark-on reclaims are carried out to 1 sample of Sishen wan.To psoralen, Isopsoralen, Dehydrodiisoeugenol, Schisandra chinensis
Alcohol first, rutaecarpin and Rutaecarpine 6 substances, are separately added into standard items corresponding to 0.5,1.0 and 1.5 times of measured amount
Content calculates its recovery of standard addition.It the results are shown in Table 4.The result shows that this method recovery of standard addition is between 92.6-107.5, RSD
Less than 5.32%.
4 Sishen wan sample mark-on reclaims result of table
Claims (5)
1. a kind of flash distillation gas chromatography measures psoralen in Sishen wan, Isopsoralen, Dehydrodiisoeugenol, five simultaneously
The method of taste alcohol first, rutaecarpin and Rutaecarpine, which is characterized in that the method are as follows:
(1) flash distillation gas chromatography detection Sishen wan sample obtains the qualitative analysis
Sishen wan sample is ground into powder and is fitted into cracker, cracker is placed at gas chromatograph injection port, when splitting
Sample introduction when solution device temperature reaches 300~350 DEG C, is detected with gas chromatograph, obtains gas chromatogram, pass through contrast standard substance
Retention time obtains psoralen, Isopsoralen, Dehydrodiisoeugenol, schizandrin, evodia rutaecarpa in Sishen wan sample
The qualitative analysis of alkali and Rutaecarpine；
The testing conditions of the gas chromatograph are as follows: chromatographic column is TRB-5 quartz capillary column, and column temperature rise program is initial temperature 50
DEG C, be raised to 200 DEG C with 5~10 DEG C/min rate, then be raised to 300 DEG C with 3~5 DEG C/min rate, then 300 DEG C keep 5~
15min；Injector temperature is 280~320 DEG C, and detector temperature is 280~320 DEG C, 30~50:1 of split ratio；Carrier gas is nitrogen
Or helium, flow velocity 1.0mL/min；
Cracker condition: 300~350 DEG C of furnace temperature of cracking；Cracker with 300~350 DEG C of gas chromatograph interface temperature；
(2) external standard method establishes standard working curve
The standard items of psoralen, Isopsoralen, schizandrin are dissolved in methylene chloride, are configured to hybrid standard product solution
I；The standard items of Dehydrodiisoeugenol, rutaecarpin, Rutaecarpine are dissolved in methylene chloride, it is molten to be configured to hybrid standard product
Liquid II；Using gas chromatograph testing conditions identical with step (1) and cracker condition, to hybrid standard product solution I, II into
Row flash distillation gas chromatography detection, obtains gas chromatogram, is cross with the concentration of each standard items in hybrid standard product solution I, II
The peak area value of each standard items is that ordinate draws standard working curve, and then obtains normal linearity in coordinate, gas chromatogram
Equation；
In the hybrid standard product solution I, psoralen, Isopsoralen, the concentration of schizandrin standard items are respectively independent
For 20~10000mg/L；
In the hybrid standard product solution II, Dehydrodiisoeugenol, rutaecarpin, Rutaecarpine standard items concentration respectively
Stand alone as 20~2000mg/L；
(3) quantitative analysis results of index ingredient in Sishen wan sample are obtained
By in the gas chromatogram of Sishen wan sample obtained by step (1), psoralen, Isopsoralen, Dehydrodiisoeugenol,
The peak area value of schizandrin, rutaecarpin and Rutaecarpine is substituted into respectively in normal linearity equation obtained by step (2), into
And the content of each index ingredient in Sishen wan sample is calculated.
2. the method as described in claim 1, which is characterized in that it is powdered that Sishen wan sample is ground into 80~120 mesh.
3. the method as described in claim 1, which is characterized in that in step (1), the testing conditions of the gas chromatograph are as follows:
Chromatographic column is TRB-5 quartz capillary column, and column temperature rise program is 50 DEG C of initial temperature, is raised to 200 DEG C with 10 DEG C/min rate, then with
5 DEG C/min rate is raised to 300 DEG C, is then 300 DEG C in 300 DEG C of holding 10min injector temperatures, and detector temperature is 300 DEG C,
30~50:1 of split ratio；Carrier gas is nitrogen or helium, flow velocity 1.0mL/min.
4. the method as described in claim 1, which is characterized in that in step (2), in the hybrid standard product solution I, psoralea corylifolia
Element, Isopsoralen, schizandrin standard items concentration respectively stand alone as 50~10000mg/L.
5. the method as described in claim 1, which is characterized in that in step (2), in the hybrid standard product solution II, dehydrogenation
Two isoeugenols, rutaecarpin, Rutaecarpine standard items concentration respectively stand alone as 50~2000mg/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710536087.8A CN107436331B (en) | 2017-07-04 | 2017-07-04 | The method for flashing index ingredient in gas chromatography measurement Sishen wan |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710536087.8A CN107436331B (en) | 2017-07-04 | 2017-07-04 | The method for flashing index ingredient in gas chromatography measurement Sishen wan |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107436331A CN107436331A (en) | 2017-12-05 |
| CN107436331B true CN107436331B (en) | 2019-11-29 |
Family
ID=60460814
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710536087.8A Active CN107436331B (en) | 2017-07-04 | 2017-07-04 | The method for flashing index ingredient in gas chromatography measurement Sishen wan |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107436331B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109507354B (en) * | 2019-01-17 | 2021-02-02 | 浙江工业大学 | Method for determining content of K powder in human hair by flash evaporation-gas chromatography-mass spectrometry |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104198634A (en) * | 2014-08-11 | 2014-12-10 | 沈阳双鼎制药有限公司 | Method for establishing Sishen tablet fingerprint spectrum |
| CN105136936A (en) * | 2015-09-18 | 2015-12-09 | 西安科技大学 | Rapid detection method for psoralen and isopsoralen |
-
2017
- 2017-07-04 CN CN201710536087.8A patent/CN107436331B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104198634A (en) * | 2014-08-11 | 2014-12-10 | 沈阳双鼎制药有限公司 | Method for establishing Sishen tablet fingerprint spectrum |
| CN105136936A (en) * | 2015-09-18 | 2015-12-09 | 西安科技大学 | Rapid detection method for psoralen and isopsoralen |
Non-Patent Citations (2)
| Title |
|---|
| Akira Katoh等.Systems Biology in a Commercial Quality Study of the Japanese Angelica Radix: Toward an Understanding of Traditional Medicinal Plants.《The American Journal of Chinese Medicine》.2011,第39卷(第4期), * |
| 陈伟等.SFE-CGC法测定四神丸中主要成分的含量.《海峡药学》.1999,第11卷(第2期), * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107436331A (en) | 2017-12-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Al-Hawasli et al. | Development of a validated HPLC method for the separation and analysis of a Bromazepam, Medazepam and Midazolam mixture | |
| CN110927311B (en) | Construction method of UPLC (ultra performance liquid chromatography) characteristic spectrum of dogbane leaf medicinal material and method for measuring content of flavonoid component of dogbane leaf medicinal material | |
| CN107436331B (en) | The method for flashing index ingredient in gas chromatography measurement Sishen wan | |
| CN106053658A (en) | Burned Rhizoma drynariae formula granule characteristic spectrum and establishing method thereof | |
| CN107064363B (en) | A method of flash distillation gas chromatography evaluates kadsura longepedunculata quality in commercially available Chinese patent drug | |
| CN103529140B (en) | Method for determining content of saffron in medicinal composition | |
| Varma et al. | Gas Chromatography-Head Space-Flame Ionization Sensor based assessment of four residuary solvents in rivaroxaban bulk medication | |
| Huzar et al. | Determination of ethanol content in medicated syrups by static headspace gas chromatography | |
| CN105486776B (en) | The gas chromatography analysis method of Metoclopramide | |
| CN106198791A (en) | Lignum Aquilariae Resinatum tetrol and the method for benzylacetone in a kind of Lignum Aquilariae Resinatum of mensuration simultaneously | |
| CN103575850A (en) | Detection method for Gymnadenia conopsea medicinal material | |
| Cao et al. | Solid-phase microextraction–gas chromatographic–mass spectrometric analysis of volatile compounds from Curcuma wenyujin YH Chen et C. Ling | |
| CN113759035A (en) | Method for constructing fingerprint of Xiaochengqi decoction | |
| CN105301123A (en) | HPLC detection method for alpinia-cyperus preparations | |
| CN104374841A (en) | Quality control reference substance for antelope's horn tablets for common cold and application of quality control reference substance | |
| CN106018625A (en) | Method for detecting eucalyptol in moxa sticks | |
| CN107843675A (en) | The method for flashing five tastes protonatomic mass in gas chromatography evaluation Chinese patent drug | |
| CN105301158A (en) | Fingerprint spectrum determination method for Simotang oral solution | |
| Pang et al. | Establishment of quantitatively analytical methods for the determination of aroma components in edible spices using a homemade chromatographic monolithic column | |
| Cai et al. | Simultaneous determination of paeonol and ferulic acid in Su-Xiao-Xin-Tong dropping pills by high performance liquid chromatography with matrix solid-phase dispersion extraction | |
| CN108226316A (en) | Method that is a kind of while measuring 7 kinds of lignanoid's contents in Schisandra chinensis | |
| Chen et al. | Quality and safety control of tumor‐shrinking decoction (TSD): A Chinese herbal preparation for the treatment of uterine fibroids | |
| Selvan et al. | Determination of ethanol content in ayurvedic formulations kumaryasava and mustakarista by gas chromatography | |
| CN108956829B (en) | Method for simultaneously determining six components in stomach-nourishing xiangsha tablets | |
| CN102253146A (en) | Determination method of eugenol content in stomach-warming and pain-relieving paste |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |