CN108680570A - A kind of quality determining method of Radix Notoginseng oral preparation - Google Patents
A kind of quality determining method of Radix Notoginseng oral preparation Download PDFInfo
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Abstract
The invention discloses the quality determining method that drug processes a kind of Radix Notoginseng oral preparation of detection technique field, which is as follows：S1：Saponin content detects；S2：Pesticide residue content detection；S3：Content of beary metal detects, the present invention can detect saponin content, content of beary metal and the Chinese medicine residual content in place Radix Notoginseng, its detection method is simple, testing result is accurate, raising for the quality of production of Radix Notoginseng oral solution provides quality assurance, the quality testing system of a perfect pseudo-ginseng can be set up, the processing for Radix Notoginseng preparation is preferred and quality improves reliable foundation.
Description
Technical field
The invention discloses a kind of quality determining methods of Radix Notoginseng oral preparation, specially drug processing detection technique neck
Domain.
Background technology
Radix Notoginseng oral solution have it is anti-ageing, righting reinforcing invigorates vital energy and reinforce the heart, and invigorating the spleen consolidates, nourishing Yin and moistening dryness, cough-relieving of promoting the production of body fluid；And have
Improve immunity of organisms, the effect of increasing leukocyte and hemochrome.Radix Notoginseng oral solution is carried out notoginsenoside and is contained in preparation process
Amount, the measurement of content of beary metal and pesticide residue content, and a set of perfect Radix Notoginseng granular mass standard is set up, can be three
The processing of seven products is preferred and the quality of Radix Notoginseng oral solution provides reliable and stable foundation.For this purpose, we have proposed one kind three
The quality determining method of seven oral preparations comes into operation, to solve the above problems.
Invention content
The purpose of the present invention is to provide a kind of quality determining methods of Radix Notoginseng oral preparation, to solve above-mentioned background technology
The problem of middle proposition.
To achieve the above object, the present invention provides the following technical solutions：A kind of quality determining method of Radix Notoginseng oral preparation,
The detection method is as follows：
S1：Saponin content detects：Arasaponin is extracted from Radix Notoginseng oral solution sample takes 15~25mg's after dry
2~6molL is added in dry total saposins in 50~60% methanol solution-1Hydrogen chloride hydrolyzes 5~7h at 100~120 DEG C, makes
Arasaponin hydrolysis is complete, extracts aglycon with dichloromethane, evaporated under reduced pressure obtains 7~9mg of aglycon, and is dissolved in 90~95%
Ethyl alcohol in be settled to 100~120ml, as notoginsenoside sample solution；
Deionized water is added in notoginsenoside sample solution, until 150~180ml, by macroporous absorbent resin after dissolving, on
Column finishes, and washes away water-soluble sugar with the deionized water of 80~100ml, then elute soap with 90~95% 200~300ml of ethyl alcohol
Glycosides keeps 1~3mlmin-1Flow velocity, collect eluent and depressurize and volatilize, then with 100~150ml, 15~30% methanol
Dissolve and by cation exchange resin after, the methanol-eluted fractions evaporated under reduced pressure methanol of collection, take 1ml tool plug test tube develop the color
After measure its light absorption value, according to 2 times measure mean value computation arasaponin content；
S2：Pesticide residue content detection：Take the Radix Notoginseng oral solution of 2g to be placed in 100ml conical flask with cover, add water 20~
30ml soaked overnights, precision plus 30~40ml of acetone, weighed weight are ultrasonically treated 30min, and weighed weight, is used in combination acetone again
It supplies the weight of less loss, adds 6~8g of sodium chloride, precision addition 20~30ml of dichloromethane, weighed weight, it is ultrasonically treated 15~
30min, weighed weight, the weight of less loss, 10000~15000rmin are supplied with dichloromethane again-15~7min is centrifuged, it will
Organic phase moves into the 100ml conical flask with cover equipped with appropriate anhydrous sodium sulfate rapidly, stands 4~6h；
Precision measures 35~40ml, is concentrated under reduced pressure into 30~50 DEG C of water-baths and closely does, and a small amount of petroleum ether is added to repeat above-mentioned behaviour
Work is cleared to dichloromethane and acetone, with petroleum ether dissolution and is transferred in 10ml tool plug graduated centrifuge tubes, addition petroleum ether is dilute
It releases to 5~6ml, is carefully added into 1~2ml of sulfuric acid, shake 1~3min, 3000~4000rmin-110~20min is centrifuged, is taken
Clear liquid, observes the variation of chromatogram on gas chromatograph, and is compared with pesticide residue content chromatogram, to detect
Whether the pesticide residue content for going out Radix Notoginseng oral solution is up to standard；
S3：The measurement of content of beary metal：Radix Notoginseng oral solution 5~7ml of sample is weighed, is placed in counteracting tank, addition 8~
10ml nitric acid, 3~5ml hydrofluoric acid and 3~5ml hydrogen chloride, it is careful to shake so that the gas just generated discharges at once, at normal temperatures
Tank sealing is put into microwave system after 24~36h of placement and is cleared up, room temperature is then cooled to, resolution is opened in ventilated environment
Tank in sample filtering to crucible, will be placed on electric hot plate and be heated to 100~120 DEG C and catch up with acid, and liquid is through 0.4~0.5 μm after catching up with acid
Filter membrane is settled to 25ml with 2% dust technology, places spare；
Digestion solution prepared by the above process is transferred in colorimetric cylinder, is added than being settled to 25ml with deionized water after toner
It is prepared into prepare liquid, sample analysis is carried out with atomic fluorescence detector, measures its content of beary metal.
Preferably, in the step S1, the extracting method of arasaponin is：It is added 70% in Radix Notoginseng oral solution sample
Ethyl alcohol, it is 1 that the addition of feed liquid, which is compared,:12, it is extracted 4 times at high frequency 50KHZ, each ultrasound 30min, the extraction of arasaponin
Rate is 96.42%.
Preferably, in the step S2, the carrier gas of gas chromatograph is High Purity Nitrogen, and column flow rate is 1~3mlmin-1, tail
Blow 50~60mlmin-1, inlet temperature is 240~260 DEG C, and the temperature of detector is 280~300 DEG C, and sample introduction split ratio is
5:1, the process of temperature programming is 100~120 DEG C of initial temperature, 1~3min is kept, with 20 DEG C of min-1Speed be warming up to
210~230 DEG C, 1~3min is kept, then with 10~20 DEG C of min-1It is warming up to 240 DEG C of min-1260 DEG C, and holding 6~
8min。
Preferably, in the step S3, the program of resolution is to be warming up to 160~180 DEG C, and temperature-rise period is complete in 15min
At, 10~15min of holding, and taken out after cooling 5~10min.
Preferably, in the step S3, than the mixture that toner is hydrogen chloride, thiocarbamide and ascorbic acid, wherein hydrogen chloride：
Thiocarbamide：Ascorbic acid=5.5:1.6:0.8, it is 0.5 than the addition volume ratio of toner and digestion solution:1.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention can detect the saponin content, again in place Radix Notoginseng
Tenor and Chinese medicine residual content, detection method is simple, and testing result is accurate, is the quality of production of Radix Notoginseng oral solution
Raising provides quality assurance, can set up the quality testing system of a perfect pseudo-ginseng, the big gun prepared for Radix Notoginseng
System is preferably and quality improves reliable foundation.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
The every other embodiment that technical staff is obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment one
A kind of quality determining method of Radix Notoginseng oral preparation, the detection method are as follows：
S1：Saponin content detects：Arasaponin is extracted from Radix Notoginseng oral solution sample takes the drying of 15mg after dry
2molL is added in 50% methanol solution in total saposins-1Hydrogen chloride hydrolyzes 5h at 100 DEG C, keeps arasaponin hydrolysis complete,
Aglycon is extracted with dichloromethane, evaporated under reduced pressure obtains aglycon 7mg, and is dissolved in 90% ethyl alcohol and is settled to 100ml, as three
The carrier gas of seven saponin(e sample solution gas chromatographs is High Purity Nitrogen, column flow rate 1mlmin-1, tail blows 50mlmin-1, charging
Mouth temperature is 240 DEG C, and the temperature of detector is 280 DEG C, and sample introduction split ratio is 5:1, the process of temperature programming is initial temperature
100 DEG C, 1min is kept, with 20 DEG C of min-1Speed be warming up to 210 DEG C, keep 1min, then with 10 DEG C of min-1It is warming up to
240℃·min-1260 DEG C, and keep 6min；
Deionized water is added in notoginsenoside sample solution, until 150ml, by macroporous absorbent resin after dissolving, upper prop is complete
Finish, water-soluble sugar is washed away with the deionized water of 80ml, then saponin(e is eluted with 90% ethyl alcohol 200ml, keep 1mlmin-1Stream
Speed, collect eluent and depressurize volatilize, then with 100ml, 15% methanol dissolve and by cation exchange resin after, collection
Methanol-eluted fractions evaporated under reduced pressure methanol takes 1ml to measure its light absorption value after tool plug test tube colour developing, the mean value measured according to 2 times
Calculate the content of arasaponin；
S2：Pesticide residue content detection：It takes the Radix Notoginseng oral solution of 2g to be placed in 100ml conical flask with cover, water 20ml is added to soak
Overnight, precision plus acetone 30ml, weighed weight are ultrasonically treated 30min to bubble, and weighed weight, is used in combination acetone to supply less loss again
Weight, adds sodium chloride 6g, precision addition dichloromethane 20ml, and weighed weight is ultrasonically treated 15min, again weighed weight, uses
Dichloromethane supplies the weight of less loss, 10000rmin-15min is centrifuged, organic phase is moved into rapidly, appropriate anhydrous slufuric acid is housed
In the 100ml conical flask with cover of sodium, 4h is stood；The carrier gas of gas chromatograph is High Purity Nitrogen, column flow rate 1mlmin-1, tail blows
50ml·min-1, inlet temperature is 240 DEG C, and the temperature of detector is 280 DEG C, and sample introduction split ratio is 5:1, temperature programming
Process is 100 DEG C of initial temperature, 1min is kept, with 20 DEG C of min-1Speed be warming up to 210 DEG C, keep 1min, then with 10
℃·min-1It is warming up to 240 DEG C of min-1260 DEG C, and keep 6min；
Precision measures 35ml, is concentrated under reduced pressure into 30 DEG C of water-baths and closely does, a small amount of petroleum ether is added to repeat aforesaid operations to dichloro
Methane and acetone are cleared, with petroleum ether dissolution and are transferred in 10ml tool plug graduated centrifuge tubes, and addition petroleum ether is diluted to 5ml,
It is carefully added into sulfuric acid 1ml, shakes 1min, 3000rmin-110min is centrifuged, supernatant is taken, chromatography is observed on gas chromatograph
The variation of figure, and be compared with pesticide residue content chromatogram, to detect the pesticide residue content of Radix Notoginseng oral solution
It is whether up to standard；
S3：The measurement of content of beary metal：Radix Notoginseng oral solution sample 5ml is weighed, is placed in counteracting tank, addition 8ml nitric acid,
3ml hydrofluoric acid and 3ml hydrogen chloride, it is careful to shake so that the gas just generated discharges at once, it places at normal temperatures afterwards that tank is close for 24 hours
Envelope, which is put into microwave system, to be cleared up, and is then cooled to room temperature, counteracting tank is opened in ventilated environment, by sample filtering to crucible
In, it is placed on electric hot plate and is heated to 100 DEG C and catches up with acid, liquid is settled to 25ml with 2% dust technology, puts through 0.4 μm of filter membrane after catching up with acid
It purchases use；The program of resolution is to be warming up to 160 DEG C, and temperature-rise period is completed in 15min, keeps 10min, and taken after cooling 5min
Go out；
Digestion solution prepared by the above process is transferred in colorimetric cylinder, is added than being settled to 25ml with deionized water after toner
Be prepared into prepare liquid, carry out sample analysis with atomic fluorescence detector, measure its content of beary metal, than toner be hydrogen chloride, thiocarbamide and
The mixture of ascorbic acid, wherein hydrogen chloride：Thiocarbamide：Ascorbic acid=5.5:1.6:0.8, than the addition body of toner and digestion solution
Product is than being 0.5:1.
Embodiment two
A kind of quality determining method of Radix Notoginseng oral preparation, the detection method are as follows：
S1：Saponin content detects：Arasaponin is extracted from Radix Notoginseng oral solution sample takes the drying of 25mg after dry
6molL is added in 60% methanol solution in total saposins-1Hydrogen chloride hydrolyzes 7h at 120 DEG C, keeps arasaponin hydrolysis complete,
Aglycon is extracted with dichloromethane, evaporated under reduced pressure obtains aglycon 9mg, and is dissolved in 95% ethyl alcohol and is settled to 120ml, as three
The carrier gas of seven saponin(e sample solution gas chromatographs is High Purity Nitrogen, column flow rate 3mlmin-1, tail blows 60mlmin-1, charging
Mouth temperature is 260 DEG C, and the temperature of detector is 300 DEG C, and sample introduction split ratio is 5:1, the process of temperature programming is initial temperature
120 DEG C, 3min is kept, with 20 DEG C of min-1Speed be warming up to 230 DEG C, keep 3min, then with 20 DEG C of min-1It is warming up to
240℃·min-1260 DEG C, and keep 8min；
Deionized water is added in notoginsenoside sample solution, until 180ml, by macroporous absorbent resin after dissolving, upper prop is complete
Finish, water-soluble sugar is washed away with the deionized water of 100ml, then saponin(e is eluted with 95% ethyl alcohol 300ml, keep 3mlmin-1's
Flow velocity, collect eluent and depressurize volatilize, then with 150ml, 30% methanol dissolving and by cation exchange resin after, collection
Methanol-eluted fractions evaporated under reduced pressure methanol, take 1ml tool plug test tube colour developing after measure its light absorption value, according to 2 times measure it is equal
Value calculates the content of arasaponin；
S2：Pesticide residue content detection：It takes the Radix Notoginseng oral solution of 2g to be placed in 100ml conical flask with cover, water 30ml is added to soak
Overnight, precision plus acetone 40ml, weighed weight are ultrasonically treated 30min to bubble, and weighed weight, is used in combination acetone to supply less loss again
Weight, adds sodium chloride 8g, precision addition dichloromethane 30ml, and weighed weight is ultrasonically treated 30min, again weighed weight, uses
Dichloromethane supplies the weight of less loss, 15000rmin-17min is centrifuged, organic phase is moved into rapidly, appropriate anhydrous slufuric acid is housed
In the 100ml conical flask with cover of sodium, 6h is stood；The carrier gas of gas chromatograph is High Purity Nitrogen, column flow rate 3mlmin-1, tail blows
60ml·min-1, inlet temperature is 260 DEG C, and the temperature of detector is 300 DEG C, and sample introduction split ratio is 5:1, temperature programming
Process is 120 DEG C of initial temperature, 3min is kept, with 20 DEG C of min-1Speed be warming up to 230 DEG C, keep 3min, then with 20
℃·min-1It is warming up to 240 DEG C of min-1260 DEG C, and keep 8min；
Precision measures 40ml, is concentrated under reduced pressure into 50 DEG C of water-baths and closely does, a small amount of petroleum ether is added to repeat aforesaid operations to dichloro
Methane and acetone are cleared, with petroleum ether dissolution and are transferred in 10ml tool plug graduated centrifuge tubes, and addition petroleum ether is diluted to 6ml,
It is carefully added into sulfuric acid 2ml, shakes 3min, 4000rmin-120min is centrifuged, supernatant is taken, chromatography is observed on gas chromatograph
The variation of figure, and be compared with pesticide residue content chromatogram, to detect the pesticide residue content of Radix Notoginseng oral solution
It is whether up to standard；
S3：The measurement of content of beary metal：Radix Notoginseng oral solution sample 7ml is weighed, is placed in counteracting tank, 10ml nitre is added
Acid, 5ml hydrofluoric acid and 5ml hydrogen chloride, careful to shake so that the gas just generated discharges at once, placing at normal temperatures will after 36h
Tank sealing, which is put into microwave system, clears up, and is then cooled to room temperature, counteracting tank is opened in ventilated environment, by sample filtering to earthenware
In crucible, it is placed on electric hot plate and is heated to 120 DEG C and catches up with acid, liquid is settled to 25ml through 0.5 μm of filter membrane with 2% dust technology after catching up with acid,
It places spare；The program of resolution is to be warming up to 180 DEG C, and temperature-rise period is completed in 15min, keeps 15min, and cooling 10min
After take out；
Digestion solution prepared by the above process is transferred in colorimetric cylinder, is added than being settled to 25ml with deionized water after toner
Be prepared into prepare liquid, carry out sample analysis with atomic fluorescence detector, measure its content of beary metal, than toner be hydrogen chloride, thiocarbamide and
The mixture of ascorbic acid, wherein hydrogen chloride：Thiocarbamide：Ascorbic acid=5.5:1.6:0.8, than the addition body of toner and digestion solution
Product is than being 0.5:1.
Embodiment three
A kind of quality determining method of Radix Notoginseng oral preparation, the detection method are as follows：
S1：Saponin content detects：Arasaponin is extracted from Radix Notoginseng oral solution sample takes the drying of 20mg after dry
4molL is added in 55% methanol solution in total saposins-1Hydrogen chloride hydrolyzes 6h at 110 DEG C, keeps arasaponin hydrolysis complete,
Aglycon is extracted with dichloromethane, evaporated under reduced pressure obtains aglycon 8mg, and is dissolved in 94% ethyl alcohol and is settled to 110ml, as three
The carrier gas of seven saponin(e sample solution gas chromatographs is High Purity Nitrogen, column flow rate 2mlmin-1, tail blows 55mlmin-1, charging
Mouth temperature is 250 DEG C, and the temperature of detector is 290 DEG C, and sample introduction split ratio is 5:1, the process of temperature programming is initial temperature
110 DEG C, 2min is kept, with 20 DEG C of min-1Speed be warming up to 220 DEG C, keep 2min, then with 16 DEG C of min-1It is warming up to
240℃·min-1260 DEG C, and keep 7min；
Deionized water is added in notoginsenoside sample solution, until 160ml, by macroporous absorbent resin after dissolving, upper prop is complete
Finish, water-soluble sugar is washed away with the deionized water of 90ml, then saponin(e is eluted with 93% ethyl alcohol 260ml, keep 2mlmin-1Stream
Speed, collect eluent and depressurize volatilize, then with 130ml, 25% methanol dissolve and by cation exchange resin after, collection
Methanol-eluted fractions evaporated under reduced pressure methanol takes 1ml to measure its light absorption value after tool plug test tube colour developing, the mean value measured according to 2 times
Calculate the content of arasaponin；
S2：Pesticide residue content detection：It takes the Radix Notoginseng oral solution of 2g to be placed in 100ml conical flask with cover, water 25ml is added to soak
Overnight, precision plus acetone 35ml, weighed weight are ultrasonically treated 30min to bubble, and weighed weight, is used in combination acetone to supply less loss again
Weight, adds sodium chloride 7g, precision addition dichloromethane 25ml, and weighed weight is ultrasonically treated 20min, again weighed weight, uses
Dichloromethane supplies the weight of less loss, 13000rmin-16min is centrifuged, organic phase is moved into rapidly, appropriate anhydrous slufuric acid is housed
In the 100ml conical flask with cover of sodium, 5h is stood；The carrier gas of gas chromatograph is High Purity Nitrogen, column flow rate 2mlmin-1, tail blows
55ml·min-1, inlet temperature is 250 DEG C, and the temperature of detector is 290 DEG C, and sample introduction split ratio is 5:1, temperature programming
Process is 110 DEG C of initial temperature, 2min is kept, with 20 DEG C of min-1Speed be warming up to 220 DEG C, keep 2min, then with 15
℃·min-1It is warming up to 240 DEG C of min-1260 DEG C, and keep 7min；
Precision measures 38ml, is concentrated under reduced pressure into 40 DEG C of water-baths and closely does, a small amount of petroleum ether is added to repeat aforesaid operations to dichloro
Methane and acetone are cleared, with petroleum ether dissolution and are transferred in 10ml tool plug graduated centrifuge tubes, and addition petroleum ether is diluted to 5ml,
It is carefully added into sulfuric acid 1ml, shakes 2min, 3500rmin-115min is centrifuged, supernatant is taken, chromatography is observed on gas chromatograph
The variation of figure, and be compared with pesticide residue content chromatogram, to detect the pesticide residue content of Radix Notoginseng oral solution
It is whether up to standard；
S3：The measurement of content of beary metal：Radix Notoginseng oral solution sample 6ml is weighed, is placed in counteracting tank, addition 9ml nitric acid,
4ml hydrofluoric acid and 4ml hydrogen chloride, it is careful to shake so that the gas just generated discharges at once, it places at normal temperatures tank is close after 30h
Envelope, which is put into microwave system, to be cleared up, and is then cooled to room temperature, counteracting tank is opened in ventilated environment, by sample filtering to crucible
In, it being placed on electric hot plate and is heated to 110 DEG C and catches up with acid, liquid is settled to 25ml through 0.45 μm of filter membrane with 2% dust technology after catching up with acid,
It places spare；The program of resolution is to be warming up to 170 DEG C, and temperature-rise period is completed in 15min, keeps 14min, and after cooling 8min
It takes out；
Digestion solution prepared by the above process is transferred in colorimetric cylinder, is added than being settled to 25ml with deionized water after toner
Be prepared into prepare liquid, carry out sample analysis with atomic fluorescence detector, measure its content of beary metal, than toner be hydrogen chloride, thiocarbamide and
The mixture of ascorbic acid, wherein hydrogen chloride：Thiocarbamide：Ascorbic acid=5.5:1.6:0.8, than the addition body of toner and digestion solution
Product is than being 0.5:1.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (5)
1. a kind of quality determining method of Radix Notoginseng oral preparation, it is characterised in that：The detection method is as follows：
S1：Saponin content detects：Arasaponin is extracted from Radix Notoginseng oral solution sample takes the drying of 15~25mg after dry
2~6molL is added in total saposins in 50~60% methanol solution-1Hydrogen chloride hydrolyzes 5~7h at 100~120 DEG C, makes Radix Notoginseng
Total saposins hydrolysis is complete, extracts aglycon with dichloromethane, evaporated under reduced pressure obtains 7~9mg of aglycon, and is dissolved in 90~95% second
100~120ml is settled in alcohol, as notoginsenoside sample solution；
Deionized water is added in notoginsenoside sample solution, until 150~180ml, by macroporous absorbent resin after dissolving, upper prop is complete
Finish, water-soluble sugar is washed away with the deionized water of 80~100ml, then saponin(e is eluted with 90~95% 200~300ml of ethyl alcohol, protected
Hold 1~3mlmin-1Flow velocity, collect eluent and depressurize volatilize, then with 100~150ml, 15~30% methanol dissolve simultaneously
After cation exchange resin, the methanol-eluted fractions evaporated under reduced pressure methanol of collection takes 1ml to be measured after tool plug test tube colour developing
Its light absorption value, the content of the mean value computation arasaponin measured according to 2 times；
S2：Pesticide residue content detection：It takes the Radix Notoginseng oral solution of 2g to be placed in 100ml conical flask with cover, 20~30ml of water is added to soak
Overnight, precision plus 30~40ml of acetone, weighed weight are ultrasonically treated 30min to bubble, and weighed weight, is used in combination acetone to supply and subtracts again
The weight of mistake adds 6~8g of sodium chloride, precision addition 20~30ml of dichloromethane, and weighed weight is ultrasonically treated 15~30min,
Weighed weight again supplies the weight of less loss, 10000~15000rmin with dichloromethane-15~7min is centrifuged, by organic phase
It is rapid to move into the 100ml conical flask with cover equipped with appropriate anhydrous sodium sulfate, stand 4~6h；
Precision measures 35~40ml, is concentrated under reduced pressure into 30~50 DEG C of water-baths and closely does, a small amount of petroleum ether is added to repeat aforesaid operations extremely
Dichloromethane and acetone are cleared, with petroleum ether dissolution and are transferred in 10ml tool plug graduated centrifuge tubes, addition petroleum ether is diluted to 5
~6ml is carefully added into 1~2ml of sulfuric acid, shakes 1~3min, 3000~4000rmin-110~20min is centrifuged, supernatant is taken,
The variation of chromatogram is observed on gas chromatograph, and is compared with pesticide residue content chromatogram, to detect three
Whether the pesticide residue content of seven oral solutions is up to standard；
S3：The measurement of content of beary metal：Radix Notoginseng oral solution 5~7ml of sample is weighed, is placed in counteracting tank, 8~10ml nitre is added
Acid, 3~5ml hydrofluoric acid and 3~5ml hydrogen chloride, it is careful to shake so that the gas just generated discharges at once, 24 are placed at normal temperatures
Tank sealing is put into microwave system after~36h and is cleared up, room temperature is then cooled to, counteracting tank is opened in ventilated environment, by sample
Product are filtered into crucible, are placed on electric hot plate and are heated to 100~120 DEG C and catch up with acid, and liquid is used through 0.4~0.5 μm of filter membrane after catching up with acid
2% dust technology is settled to 25ml, places spare；
Digestion solution prepared by the above process is transferred in colorimetric cylinder, is added and is prepared than being settled to 25ml with deionized water after toner
At prepare liquid, sample analysis is carried out with atomic fluorescence detector, measures its content of beary metal.
2. a kind of quality determining method of Radix Notoginseng oral preparation according to claim 1, it is characterised in that：The step S1
In, the extracting method of arasaponin is：70% ethyl alcohol is added in Radix Notoginseng oral solution sample, it is 1 that the addition of feed liquid, which is compared,:
12, it is extracted 4 times at high frequency 50KHZ, each ultrasound 30min, the recovery rate of arasaponin is 96.42%.
3. a kind of quality determining method of Radix Notoginseng oral preparation according to claim 1, it is characterised in that：The step S2
In, the carrier gas of gas chromatograph is High Purity Nitrogen, and column flow rate is 1~3mlmin-1, tail blows 50~60mlmin-1, feed inlet temperature
Degree is 240~260 DEG C, and the temperature of detector is 280~300 DEG C, and sample introduction split ratio is 5:1, the process of temperature programming is first
100~120 DEG C of beginning temperature keeps 1~3min, with 20 DEG C of min-1Speed be warming up to 210~230 DEG C, keep 1~3min,
Again with 10~20 DEG C of min-1It is warming up to 240 DEG C of min-1260 DEG C, and keep 6~8min.
4. a kind of quality determining method of Radix Notoginseng oral preparation according to claim 1, it is characterised in that：The step S3
In, the program of resolution is to be warming up to 160~180 DEG C, and temperature-rise period is completed in 15min, 10~15min of holding, and cooling 5~
It is taken out after 10min.
5. a kind of quality determining method of Radix Notoginseng oral preparation according to claim 1, it is characterised in that：The step S3
In, than the mixture that toner is hydrogen chloride, thiocarbamide and ascorbic acid, wherein hydrogen chloride：Thiocarbamide：Ascorbic acid=5.5:1.6:
0.8, it is 0.5 than the addition volume ratio of toner and digestion solution:1.
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