CN106226447A - The quality determining method of the chest stuffiness relieving aerosol - Google Patents
The quality determining method of the chest stuffiness relieving aerosol Download PDFInfo
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- CN106226447A CN106226447A CN201610776518.3A CN201610776518A CN106226447A CN 106226447 A CN106226447 A CN 106226447A CN 201610776518 A CN201610776518 A CN 201610776518A CN 106226447 A CN106226447 A CN 106226447A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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Abstract
The invention discloses the quality determining method of a kind of the chest stuffiness relieving aerosol, described quality determining method is hexadecane or the naphthalene gas chromatography as object of reference.The detection method of the present invention is conducive to detection Oleum Santali albi composition, thus the beneficially quality control of the chest stuffiness relieving aerosol and the control of clinical efficacy.
Description
Technical field
The present invention relates to the quality determining method of a kind of Traditional Chinese medicinal aerosol.
Background technology
The chest stuffiness relieving aerosol is based on " aromatic herbs activating YANG " the theoretical Traditional Chinese medicinal aerosol developed of " to lead to for mending, to lead to ",
Effective prescription of quick-acting antalgesic for the treatment of coronary heart diseases and angina pectoris, its key component include Oleum Asari, Oleum Santali albi, Rhizoma Alpiniae Officinarum oil,
Fructus Piperis Longi oil and Borneolum Syntheticum, function activating YANG with pungent and warm drugs, regulating QI to relieve pain, for the thoracic obstruction caused by YIN-cold retardance, mechanism of qi closing, card is shown in the heart uncomfortable in chest
Bitterly, coldness of the body with chills, coronary heart diseases and angina pectoris is shown in above-mentioned disease person.The chest stuffiness relieving aerosol is volatile oil due to key component, molecularly
State is distributed, it is possible to being quickly absorbed by the body into blood, dilating coronary blood vessel, significantly improve myocardial ischemia, rapid recovery is uncomfortable in chest, breast
Bitterly, cardiopalmus, breathe hard, the angina pectoris symptom such as weak, have no drug resistance simultaneously, untoward reaction is few, safety is high.
At present, the quality testing of the chest stuffiness relieving aerosol uses gas chromatography, its characteristic spectrum and content assaying method all with
The record of " Chinese Pharmacopoeia version in 2015 " (page 1411～1413, under the chest stuffiness relieving aerosol item) is as the criterion, wherein using eucalyptol as
Object of reference, the assay method of characteristic spectrum is: with the quartzy capillary that 5% diphenyl-95% dimethyl polysiloxane is fixing phase
Tubing string (column length is 30m, and internal diameter is 0.32mm, and film thickness is 0.25 μm)；Column temperature is temperature programming: initial temperature is 65 DEG C, protects
Hold 5 minutes, with the ramp of 5 DEG C/min to 135 DEG C, keep 5 minutes, with the ramp of 1 DEG C/min to 135, keep 5 points
Clock, with the ramp of 2.5 DEG C per minute to 160 DEG C, keeps 5 minutes, with the ramp of 0.5 DEG C/min to 162 DEG C, keeps
5 minutes, then with the ramp of 6 DEG C per minute to 250 DEG C.Injector temperature is 240 DEG C, and detector temperature is 250 DEG C；Shunting
Sample introduction, split ratio is 20:1.Number of theoretical plate is calculated by eucalyptol peak should be not less than 100000.This assay method lays particular emphasis on and obtains
Characteristic spectrum Component seperation comprehensive, i.e. lays particular emphasis in the chest stuffiness relieving aerosol medicinal liquid the aobvious of the characteristic peak of component in every kind of raw material
Show, but the attention rate for the characteristic peak of preparation effectiveness is inadequate, be therefore unfavorable for controlling the Clinical efficacy of preparation.It addition,
This Gas Chromatographic Method uses eucalyptol as object of reference, and this object of reference is the component contained in preparation, and appearance time
Relatively early, it is unfavorable for realizing each characteristic peak is accurately positioned.
Summary of the invention
Present inventor is sent out for overall curative effect by each raw material components in further investigation the chest stuffiness relieving aerosol medicinal liquid
The impact waved, finds that the curative effect of the chest stuffiness relieving aerosol is affected relatively big by the specific components in wherein Oleum Santali albi, particularly Oleum Santali albi, and
Power of influence is apparently higher than other components.Based on this, the application thinks, the quality determining method of the chest stuffiness relieving aerosol of regulation in pharmacopeia
More focus on the equilibrium of each raw material components in characteristic spectrum to show, it is impossible to control the quality of the chest stuffiness relieving aerosol well and ensure that it faces
Bed effectiveness.
Find based on this, it is an object of the invention to provide the quality determining method of a kind of the chest stuffiness relieving aerosol, this detection side
Method can effectively detect the component of Oleum Santali albi in the chest stuffiness relieving aerosol medicinal liquid, thus is conducive to accurately judging the quality of the chest stuffiness relieving aerosol
And Clinical efficacy.It is an object of the invention to be achieved through the following technical solutions:
The quality determining method of a kind of the chest stuffiness relieving aerosol, described quality determining method is that hexadecane or naphthalene are as object of reference
Gas chromatography.
Quality determining method according to the present invention, it is preferable that the GC conditions of described gas chromatography includes column temperature
Temperature programming step: initial temperature is 110 DEG C, with the ramp of 5 DEG C/min to 160 DEG C, with the ramp of 1 DEG C/min
To 166 DEG C, keep 5 minutes, with the ramp of 0.5 DEG C/min to 167 DEG C, keep 5 minutes, with the speed liter of 0.5 DEG C/min
Temperature, to 168 DEG C, keeps 2 minutes, with the ramp of 10 DEG C/min to 230 DEG C, keeps 5 minutes.
Quality determining method according to the present invention, it is preferable that described GC conditions also includes: use in substituent group and contain
There is the quartz capillary column that polysiloxanes is fixing phase of 5mol% phenyl and 95mol% methyl；Injector temperature is 240 DEG C；
Fid detector temperature is 250 DEG C；In terms of hexadecane peak, it is not less than 100000 with number of theoretical plate.
Quality determining method according to the present invention, it is preferable that described GC conditions also includes: the carrier gas of employing is selected from
Nitrogen, helium, carbon dioxide or hydrogen；Flow rate of carrier gas is per minute 0.4～0.8ml；Carrier gas uses current constant mode, and split ratio is
20:1。
Quality determining method according to the present invention, it is preferable that described quality determining method comprises the following specific steps that:
(1) preparation of object of reference solution: hexadecane or naphthalene are dissolved in solvent as object of reference, molten to form object of reference
Liquid；
(2) preparation of need testing solution: use described object of reference solution that the chest stuffiness relieving aerosol medicinal liquid is diluted 3～10 times, with
Form need testing solution；
(3) gas chromatographic detection step: described need testing solution injection gas chromatography instrument is detected.
Quality determining method according to the present invention, it is preferable that in step (1), described solvent is selected from dehydrated alcohol or acetic acid
Ethyl ester；The concentration of described object of reference solution is 0.5～5 μ g objects of reference/ml.
Quality determining method according to the present invention, it is preferable that the concentration of described object of reference solution be 1～2 μ g objects of reference/
ml。
Quality determining method according to the present invention, it is preferable that in step (2), the multiple of described dilution is 6.67～7.00
Times.
Quality determining method according to the present invention, it is preferable that described quality determining method comprises the following specific steps that:
(1) preparation of object of reference solution: being mixed with dehydrated alcohol by hexadecane to form concentration is 1 μ g hexadecane/ml
Object of reference solution；
(2) preparation of need testing solution: use described object of reference solution to be diluted to by the chest stuffiness relieving aerosol medicinal liquid of 1.5ml
10ml；
(3) by the described need testing solution injection gas chromatography instrument of 1.0 μ l；GC conditions is as follows:
Using with the polysiloxanes containing 5mol% phenyl and 95mol% methyl in substituent group is the quartzy capillary fixing phase
Tubing string；With nitrogen as carrier gas, flow rate of carrier gas is 0.6ml/min, and carrier gas uses current constant mode, and split ratio is 20:1；
Column temperature is temperature programming: initial temperature is 110 DEG C, with the ramp of 5 DEG C/min to 160 DEG C, with 1 DEG C/min's
Ramp, to 166 DEG C, keeps 5 minutes, with the ramp of 0.5 DEG C/min to 167 DEG C, keeps 5 minutes, with 0.5 DEG C/min
Ramp to 168 DEG C, keep 2 minutes, with the ramp of 10 DEG C/min to 230 DEG C, keep 5 minutes；With
Injector temperature is 240 DEG C；Fid detector temperature is 250 DEG C；Number of theoretical plate is not less than in terms of hexadecane peak
100000。
Quality determining method according to the present invention, it is preferable that by being 1.390 in relative retention time in gas chromatogram
With the quality that whether existing characteristics peak, the assigned position of 1.420 judges described the chest stuffiness relieving aerosol；Wherein, described relative reservation
Ratio between the retention time of the retention time of the characteristic peak of the chest stuffiness relieving aerosol described in time representation and the characteristic peak of object of reference,
There is the deviation of ± 5% in described assigned position.
Compared with existing pharmacopeia detection method, the quality determining method of the present invention has been given prominence to the key points the chest stuffiness relieving Aerosol Characteristics
The characteristic peak of component in Oleum Santali albi in collection of illustrative plates, thus it is more beneficial for the quality control of the chest stuffiness relieving aerosol and the control of clinical efficacy.
It addition, the quality determining method of the present invention select hexadecane or naphthalene as object of reference, particularly select hexadecane as object of reference,
The location of the characteristic peak of component in the chest stuffiness relieving aerosol is easier to.
Accompanying drawing explanation
Fig. 1 is the collection of illustrative plates of the dehydrated alcohol of embodiment 1.
Fig. 2 is the collection of illustrative plates of the object of reference solution of embodiment 1.
Fig. 3 is the characteristic spectrum of the need testing solution of embodiment 1.
Fig. 4 is the characteristic spectrum of the Oleum Santali albi of comparative example 1.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to
This.
In the present invention, described " contains the polysiloxanes of 5mol% phenyl and 95mol% methyl for fixing phase in substituent group
Quartz capillary column ", in this area, also commonly referred to as " 5% diphenyl-95% dimethyl polysiloxane is the quartz of fixing phase
Capillary column ", the two has identical implication, can arbitrarily exchange use.
Conventionally, in the chest stuffiness relieving aerosol, Oleum Asari is monarch drug, and Rhizoma Alpiniae Officinarum oil, Fructus Piperis Longi oil and Oleum Santali albi are ministerial drug, and
Borneolum Syntheticum is as adjuvant drug.And present inventor is by further investigation, find that wherein the entirety of the chest stuffiness relieving aerosol is faced by Oleum Santali albi
The impact that bed curative effect plays is maximum, and two kinds of special components the most therein are bigger on the impact of preparation curative effect.Based on this, this
The characteristic spectrum that the quality determining method of the chest stuffiness relieving aerosol that invention provides obtains can be given prominence to the key points the component of Oleum Santali albi, from
And be conducive to controlling the clinical efficacy of said preparation.
The quality determining method of the chest stuffiness relieving aerosol of the present invention is using hexadecane or naphthalene as the gas chromatography of object of reference.
The quality determining method of the present invention can include the preparation process of object of reference solution, the preparation process of need testing solution and gas phase color
Spectrum detecting step.
Consisting of of the chest stuffiness relieving aerosol medicinal liquid of the present invention: the 140ml Han volatile oil in 625ml medicinal liquid, wherein Oleum Asari: wingceltis
Oleum sesami: Rhizoma Alpiniae Officinarum oil: Fructus Piperis Longi oil=23:70:32:15 (volume ratio is ml), Borneolum Syntheticum 22.5g, remaining as dehydrated alcohol.Should
The chest stuffiness relieving aerosol medicinal liquid can be available from commercially available prod, it is also possible to prepares voluntarily.When preparing voluntarily, each raw material all should meet
The standard that " Chinese Pharmacopoeia version in 2015 " (page 1411～1413, under the chest stuffiness relieving aerosol item) is recorded, and according to Chinese Pharmacopoeia
Version in 2015 " prepared by (page 1411～1413, under the chest stuffiness relieving aerosol item) preparation method of recording.
In the preparation process of the object of reference solution of the present invention, it is preferred to use hexadecane or naphthalene are as object of reference, in order to realize
Characteristic peak is positioned.According to one preferred embodiment of the invention, described object of reference uses hexadecane.The application sends out
Existing, when using hexadecane or naphthalene as object of reference, the appearance time of object of reference is suitable, is conducive to entering the characteristic peak of test sample
Row location；Wherein, the appearance time of the appearance time of hexadecane and the characteristic component of need testing solution closer to, and will not be to confession
The characteristic peak of test product causes miscellaneous peak to disturb, and is therefore more suitable for object of reference.The specifically side of preparation of the object of reference solution of the present invention
Method, by object of reference reference substance solvent dilution to suitable concentration, such as, can make the object of reference of 0.5～5 μ g objects of reference/ml
Solution, the object of reference solution of more preferably 0.5～2 μ g objects of reference/ml, is further preferably the object of reference solution of 1 μ g object of reference/ml.
Described solvent can be dehydrated alcohol, ethyl acetate etc., it is preferred to use dehydrated alcohol.According to one preferred embodiment party of the present invention
Formula, the preparation method of described object of reference is: hexadecane is appropriate, and it is molten that addition dehydrated alcohol makes 1 μ g hexadecane/ml object of reference
Liquid.
In the preparation process of the need testing solution of the present invention, can by the chest stuffiness relieving aerosol medicinal liquid solvent dilution the most again
Number.Described solvent is above-mentioned object of reference solution.Described extension rate can be 3～10 times, more preferably 5～7 times, further preferably
It it is 6.67～7.00 times.According to one preferred embodiment of the invention, the preparation method of described need testing solution is: will
1.5ml the chest stuffiness relieving aerosol medicinal liquid object of reference solution is diluted to 10ml.Or use different the chest stuffiness relieving aerosol medicinal liquid consumptions same
Dilution proportion, such as, be diluted to 20ml by 3ml the chest stuffiness relieving aerosol medicinal liquid object of reference solution.
In the gas chromatographic detection step of the present invention, need testing solution injection gas chromatography instrument is obtained characteristic spectrum.Excellent
Selection of land, the sample size of need testing solution is 1.0 μ l.
In the gas chromatographic detection step of the present invention, it is preferable that described gas chromatographic detection step also includes object of reference
The solvent injection gas chromatography instrument of solution.Preferably, the sample size of described solvent is 1.0 μ l.Preferably, described solvent is anhydrous
Ethanol.After described solvent injection gas chromatography instrument, the position of this solvent peak can be positioned, in order to avoid this solvent peak mistake being considered
The component characteristics peak of the chest stuffiness relieving aerosol, thus eliminate the interference of solvent peak.
The GC conditions of the present invention includes: the temperature programming step of column temperature: initial temperature is 110 DEG C, with 5 DEG C/min
Ramp to 160 DEG C, the ramp of 1 DEG C/min to 166 DEG C, keep 5 minutes, the ramp of 0.5 DEG C/min to 167
DEG C, keep 5 minutes, the ramp of 0.5 DEG C/min to 168 DEG C, keep 2 minutes, the ramp of 10 DEG C/min to 230 DEG C,
Keep 5 minutes.
In the GC conditions of the present invention, using with 5% diphenyl-95% dimethyl polysiloxane is the stone fixing phase
English capillary column.Described 5% diphenyl-95% dimethyl polysiloxane is that the quartz capillary column of fixing phase can use ability
Conventional those in territory, such as Agilent (Agilent) HP-5 quartz capillary column (30m × 0.32mm × 0.25 μm) etc..
In the GC conditions of the present invention, it is preferable that the carrier gas of employing can be nitrogen, helium, carbon dioxide or hydrogen
Gas, more preferably nitrogen.Preferably, flow rate of carrier gas is 0.4～0.8ml/min, more preferably 0.5～0.7ml/min, further preferably
For 0.6ml/min.Preferably, carrier gas uses current constant mode, and split ratio is 20:1.
In the GC conditions of the present invention, it is preferable that injector temperature is 240 DEG C；FID (flame ion) detector
Temperature is 250 DEG C；Number of theoretical plate is not less than 100000 in terms of hexadecane peak.
According to one preferred embodiment of the invention, described chromatographic condition is: gather with 5% diphenyl-95% dimethyl
Siloxanes is the quartz capillary column (column length is 30m, and internal diameter is 0.32mm, and film thickness is 0.25 μm) of fixing phase；Carrier gas is N2,
Flow rate of carrier gas is 0.6ml per minute, current constant mode, and split ratio is 20:1；Injector temperature is 240 DEG C；Fid detector temperature is
250℃；Column temperature is temperature programming: initial temperature is 110 DEG C, with the ramp of 5 DEG C/min to 160 DEG C, and the speed of 1 DEG C/min
It is warming up to 166 DEG C, keeps 5 minutes, the ramp of 0.5 DEG C/min to 167 DEG C, keep 5 minutes, the speed liter of 0.5 DEG C/min
Temperature, to 168 DEG C, keeps 2 minutes, the ramp of 10 DEG C/min to 230 DEG C, keeps 5 minutes；Number of theoretical plate is in terms of hexadecane peak
It is not less than 100000.
The application finds, in the gas chromatogram of the chest stuffiness relieving aerosol, relative retention time is the feature of 1.390 and 1.420
It is the most notable that the component at peak plays curative effect impact for preparation entirety.Therefore, in the present invention, by for relative retention time being
Whether existing characteristics peak, the assigned position of 1.390 and 1.420 judges the quality of described the chest stuffiness relieving aerosol.Described relative reservation
Ratio between the retention time of the retention time of the characteristic peak of the chest stuffiness relieving aerosol described in time representation and the characteristic peak of object of reference,
There is the deviation of ± 5% in described assigned position.Such as, by need testing solution injection gas chromatography instrument, form characteristic spectrum.First
Find the characteristic peak of object of reference, and determine object of reference retention time；Then object of reference retention time is multiplied by 1.390 and 1.420,
Obtain new retention time；Finally observe on new retention time position whether existing characteristics peak, thus judge described the chest stuffiness relieving
The quality of aerosol.If at existing characteristics peak, above-mentioned position, then the chest stuffiness relieving aerosol has more preferably curative effect.
Following example and comparative example use Agilent 6890N gas chromatograph；Use Agilent HP-5 quartz
Capillary column (30m × 0.32mm × 0.25 μm, with 5% diphenyl-95% dimethyl polysiloxane for fixing phase)；Ten thousand/
Balance is prunus mume (sieb.) sieb.et zucc. Teller-torr benefit (Mettler Toledo) AL204/01 type；100000/balance is prunus mume (sieb.) sieb.et zucc. Teller-torr benefit
AB135-S type；The chest stuffiness relieving aerosol is that Nanyang Pharmcy Co., Ltd., Hubei produces；The purity 99.999% of high pure nitrogen；Anhydrous second
Alcohol is analytical pure second distillation, and other reagent is analytical pure.
The preparation of the chest stuffiness relieving aerosol medicinal liquid in embodiment 1: by Oleum Asari 23ml, Oleum Santali albi 70ml, Rhizoma Alpiniae Officinarum oil 32ml, Bi
Roots of grass oil 15ml mix homogeneously, puts in 40 DEG C of water-baths, adds Borneolum Syntheticum, and slight fever makes dissolving, with dehydrated alcohol adjustment total amount to 625ml,
Mixing, filters, to obtain final product.Oleum Santali albi in comparative example 1 is identical with preparing the Oleum Santali albi used in this chest stuffiness relieving aerosol medicinal liquid.
Embodiment 1
The detection method of the chest stuffiness relieving aerosol, comprises the steps:
(1) preparation of object of reference solution: take hexadecane appropriate, adding dehydrated alcohol, to make the object of reference of 1 μ g hexadecane/ml molten
Liquid；
(2) preparation of need testing solution: precision measures 1.5ml the chest stuffiness relieving aerosol medicinal liquid, dilutes with described object of reference solution
To 10ml, obtain described need testing solution；
(3) respectively need testing solution described in object of reference solution described in 1.0 μ l dehydrated alcohol, 1.0 μ l and 1.0 μ l is injected gas
Chromatography；GC conditions is:
Use Agilent HP-5 quartz capillary column；Carrier gas is N2, flow rate of carrier gas is 0.6ml/min, current constant mode, point
Flow ratio is 20:1；Injector temperature is 240 DEG C；Fid detector temperature is 250 DEG C；Column temperature is temperature programming: initial temperature is
110 DEG C, with the ramp of 5 DEG C/min to 160 DEG C, the ramp of 1 DEG C/min to 166 DEG C, keep 5 minutes, 0.5 DEG C/min
Ramp to 167 DEG C, keep 5 minutes, the ramp of 0.5 DEG C/min to 168 DEG C, keep 2 minutes, the speed of 10 DEG C/min
Rate is warming up to 230 DEG C, keeps 5 minutes；Number of theoretical plate is not less than 100000 in terms of hexadecane peak.
Respectively obtain the gas phase collection of illustrative plates (Fig. 1) of dehydrated alcohol, the gas phase collection of illustrative plates (Fig. 2) of object of reference solution and need testing solution
Gas phase collection of illustrative plates (Fig. 3).Wherein peak S is the characteristic peak of object of reference hexadecane, peak 1～the spy that peak 8 is each component in Oleum Santali albi
Levy peak.
Comparative example 1
Except the preparation method of step (2) need testing solution being replaced with: precision measures Oleum Santali albi 0.2ml, put 10ml amount
In Ping, it is diluted to scale with above-mentioned object of reference solution, shakes up；Other conditions and step are the most same as in Example 1, obtain Fig. 4's
Oleum Santali albi component characteristics collection of illustrative plates.
In above-described embodiment 1 and comparative example 1, the retention time at each peak of Fig. 2 and Fig. 3 is as follows: object of reference peak S is
20.730min, characteristic peak 1 is 25.400min, and characteristic peak 2 is 26.016min, and characteristic peak 3 is 26.410min, and characteristic peak 4 is
26.891min, characteristic peak 5 is 28.814min, and characteristic peak 6 is 29.430min, and characteristic peak 7 is 31.788min, and characteristic peak 8 is
32.251min.The relative retention time of characteristic peak 1～8 and object of reference peak S is respectively: 1.225,1.255,1.274,1.297,
1.390,1.420,1.533,1.556, these peaks are corresponding with the peak 1 in Fig. 4～peak 8 respectively.Visible, the detection side of the present invention
Method can embody the Oleum Santali albi composition in the chest stuffiness relieving aerosol well, and characteristic peak 5 and characteristic peak 6 separating degree good.
The present invention is not limited to above-mentioned embodiment, in the case of without departing substantially from the flesh and blood of the present invention, and this area skill
Art personnel it is contemplated that any deformation, improve, replace and each fall within the scope of the present invention.
Claims (10)
1. the quality determining method of a chest stuffiness relieving aerosol, it is characterised in that described quality determining method is hexadecane or naphthalene
Gas chromatography as object of reference.
Quality determining method the most according to claim 1, it is characterised in that the GC conditions of described gas chromatography
Temperature programming step including column temperature:
Initial temperature is 110 DEG C, with the ramp of 5 DEG C/min to 160 DEG C, with the ramp of 1 DEG C/min to 166 DEG C, protects
Hold 5 minutes, with the ramp of 0.5 DEG C/min to 167 DEG C, keep 5 minutes, with the ramp of 0.5 DEG C/min to 168 DEG C,
Keep 2 minutes, with the ramp of 10 DEG C/min to 230 DEG C, keep 5 minutes.
Quality determining method the most according to claim 2, it is characterised in that described GC conditions also includes: use
In substituent group, the polysiloxanes containing 5mol% phenyl and 95mol% methyl is the quartz capillary column fixing phase；Injection port temperature
Degree is 240 DEG C；Fid detector temperature is 250 DEG C；In terms of hexadecane peak, it is not less than 100000 with number of theoretical plate.
Quality determining method the most according to claim 3, it is characterised in that described GC conditions also includes: use
Carrier gas selected from nitrogen, helium, carbon dioxide or hydrogen；Flow rate of carrier gas is per minute 0.4～0.8ml；Carrier gas uses constant current side
Formula, split ratio is 20:1.
5. according to the quality determining method described in any one of Claims 1 to 4, it is characterised in that described quality determining method
Comprise the following specific steps that:
(1) preparation of object of reference solution: hexadecane or naphthalene are dissolved in solvent as object of reference, to form object of reference solution；
(2) preparation of need testing solution: use described object of reference solution that the chest stuffiness relieving aerosol medicinal liquid is diluted 3～10 times, to be formed
Need testing solution；
(3) gas chromatographic detection step: described need testing solution injection gas chromatography instrument is detected.
Quality determining method the most according to claim 5, it is characterised in that in step (1), described solvent is selected from anhydrous second
Alcohol or ethyl acetate；The concentration of described object of reference solution is 0.5～5 μ g objects of reference/ml.
Quality determining method the most according to claim 6, it is characterised in that the concentration of described object of reference solution is 1～2 μ g
Object of reference/ml.
Quality determining method the most according to claim 5, it is characterised in that in step (2), the multiple of described dilution is
6.67～7.00 times.
Quality determining method the most according to claim 1, it is characterised in that described quality determining method includes following concrete
Step:
(1) preparation of object of reference solution: mix hexadecane with dehydrated alcohol to form the reference that concentration is 1 μ g hexadecane/ml
Thing solution；
(2) preparation of need testing solution: use described object of reference solution that the chest stuffiness relieving aerosol medicinal liquid of 1.5ml is diluted to 10ml；
(3) by the described need testing solution injection gas chromatography instrument of 1.0 μ l；GC conditions is as follows:
Using with the polysiloxanes containing 5mol% phenyl and 95mol% methyl in substituent group is the quartz capillary fixing phase
Post；With nitrogen as carrier gas, flow rate of carrier gas is 0.6ml/min, and carrier gas uses current constant mode, and split ratio is 20:1；
Column temperature is temperature programming: initial temperature is 110 DEG C, with the ramp of 5 DEG C/min to 160 DEG C, with the speed of 1 DEG C/min
It is warming up to 166 DEG C, keeps 5 minutes, with the ramp of 0.5 DEG C/min to 167 DEG C, keep 5 minutes, with the speed of 0.5 DEG C/min
Rate is warming up to 168 DEG C, keeps 2 minutes, with the ramp of 10 DEG C/min to 230 DEG C, keeps 5 minutes；With
Injector temperature is 240 DEG C；Fid detector temperature is 250 DEG C；Number of theoretical plate is not less than 100000 in terms of hexadecane peak.
10. according to Claims 1 to 4, quality determining method according to any one of 6～9, it is characterised in that by gas phase color
In spectrogram, in the assigned position that relative retention time is 1.390 and 1.420, whether existing characteristics peak is to judge described the chest stuffiness relieving aerosol
The quality of agent；Wherein, described relative retention time represents retention time and the object of reference of the characteristic peak of described the chest stuffiness relieving aerosol
Characteristic peak retention time between ratio, described assigned position exist ± 5% deviation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610776518.3A CN106226447A (en) | 2016-08-30 | 2016-08-30 | The quality determining method of the chest stuffiness relieving aerosol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610776518.3A CN106226447A (en) | 2016-08-30 | 2016-08-30 | The quality determining method of the chest stuffiness relieving aerosol |
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| Publication Number | Publication Date |
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| CN112697939A (en) * | 2020-12-23 | 2021-04-23 | 广西壮族自治区食品药品检验所 | Method for determining multiple components in wide chest aerosol based on GC-MS/MS |
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| CN112697939A (en) * | 2020-12-23 | 2021-04-23 | 广西壮族自治区食品药品检验所 | Method for determining multiple components in wide chest aerosol based on GC-MS/MS |
| CN112697939B (en) * | 2020-12-23 | 2022-04-26 | 广西壮族自治区食品药品检验所 | Method for determining multiple components in wide chest aerosol based on GC-MS/MS |
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