CN105929053A - Method for determining ephedrine hydrochloride in lung ventilating and regulating pill by using ASE-UPLC - Google Patents
Method for determining ephedrine hydrochloride in lung ventilating and regulating pill by using ASE-UPLC Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention provides a method for determining ephedrine hydrochloride in a lung ventilating and regulating pill by using ASE-UPLC. The objective of the invention is to provide the determination method which has the advantages of short extraction time, good reproducibility, complete extraction and good controllability. The method comprises the following steps: accurately weighing 1 g of a sample, placing the sample into an extraction pool with a volume of 10 mL and subjecting the sample to ester removal and extraction with n-hexane, wherein extraction temperature is 80 DEG C, static extraction time is 5 min, extraction is carried out once, and a flushing volume is 100%; then carrying out exaction again by using methanol as an extraction solvent, wherein extraction temperature is 80 DEG C, static extraction time is 8 min and extraction is carried out three times; after completion of extraction, fixing the volume of obtained extract to a constant volume of 25 mL, sucking up 1.5 mL of the extract into a 2-mL centrifuge tube filled with 300 mg of PSA, carrying out vortex treatment for 2 min, then carrying out centrifugation at a speed of 1500 r/min for 3 min and taking supernatant for ultra-high-performance liquid chromatographic analysis; and carrying out linear investigation. The method belongs to the technical field of chemical detection.
Description
Technical field
The invention discloses the assay method of a kind of ephedrine hydrochloride, specifically, be to use
ASE-UPLC measures the method for ephedrine hydrochloride in tongxuan lifei pills；Belong to chemical detection skill
Art field.
Background technology
Tongxuan lifei pills be by perilla leaf, the root of purple-flowered peucedanum, balloonflower root, semen armeniacae amarae, Chinese ephedra, Radix Glycyrrhizae,
Ten pill of making of a herb material prescription such as dried orange peel, the tuber of pinellia, taste is micro-sweet, slightly bitter, has solution
Table dissipates cold, the function that a surname's lung is only coughed, for chill bundle table, the cold cough of Lung Qi obstruction,
Disease sees heating, aversion to cold, nasal obstruction runny nose, headache, lossless, limb aching pain.Its epheday intermedia has
Have Pulvis Diaphoreticus to tremble with fear, freeing lung and relieving asthma, the effect of inducing diuresis for removing edema, for anemofrigid cold, uncomfortable in chest breath with cough,
Geomantic omen edema, its principle active component is ephedrine hydrochloride." Chinese Pharmacopoeia " version in 2015
In one regulation tongxuan lifei pills, the composition of assay is ephedrine hydrochloride.
Accelerate solvent extraction (ASE) refers in closed container in high temperature (50～200 DEG C) and height
Under the conditions of pressure (500～3000psi), at short notice, with Solvent Extract methods solid or half
The novel sample-pretreating method of one of solid sample.With ultrasonic, microwave, reflux, super face
The maturation methods such as boundary's extraction are compared, and ASE has that extractant consumption is few, extraction time is short, extraction
Take that efficiency is high, simple to operation, safety and automaticity advantages of higher.External existing
This technology is applied to the pre-treatment of sample during autonomic drug is qualitatively and quantitatively analyzed by scholar, but
In the qualitatively and quantitatively analysis of Chinese patent drug active ingredient, the pre-treating method as sample is applied
Less, the research that ephedrine hydrochloride extracts in tongxuan lifei pills has no report taste.
Summary of the invention
It is an object of the invention to provide a kind of extraction time short, and favorable reproducibility, extract completely
And the ASE-UPLC that controllability is strong measures the method for ephedrine hydrochloride in tongxuan lifei pills.
For solving above-mentioned technical problem, the technical scheme that the present invention provides is such that
A kind of ASE-UPLC measures the method for ephedrine hydrochloride in tongxuan lifei pills, includes successively
Following step:
1) accurately weighed ephedrine hydrochloride reference substance 19.77mg, by volume ratio 1:1000
Hydrochloric acid and methanol solution are settled in 50mL volumetric flask, make 0.3942g L-1Standard
Storing solution；
2) accurately weigh sample 1g to be placed in 10mL abstraction pool, with n-hexane, sample is entered
Row extracts except ester, and described Extracting temperature is 80 DEG C, and static extraction time is 5min, extracts
Number of times is 1 time, flush volume 100%, then with methyl alcohol as Extraction solvent, Extracting temperature is
80 DEG C, static extraction time is 8min, and extraction time is 3 times；Extraction will be extracted after completing
Liquid is settled to 25mL, draws 1.5mL in equipped with in the 2mL centrifuge tube of 300mg PSA,
Whirlpool 2min, 15000r/min are centrifuged 3min, take supernatant and carry out ultra high efficiency liquid phase analysis；
3) accurate absorption 0.3942g L-1Standard reserving solution 1mL, use volume ratio 1:
The hydrochloric acid of 1000 and methanol solution are settled in 25mL volumetric flask, make 0.0158g L-1
Standard liquid, sample size is respectively 0.2,0.4,0.6,0.8,1,1.2 μ L, parallel survey
Fixed 2 times, with peak area, mass concentration mg is carried out linear regression, 0.00315～
0.0189g·L-1In the range of linearity, linear equation is: Y=4184.2X+0.3465, linear phase
Close coefficients R2=0.9998.
Further, above-mentioned ASE-UPLC measures the side of ephedrine hydrochloride in tongxuan lifei pills
Method, described abstraction instrument is 350ASE.
Further, above-mentioned ASE-UPLC measures the side of ephedrine hydrochloride in tongxuan lifei pills
Method, described Ultra Performance Liquid Chromatography instrument is Agilent 1290 Ultra Performance Liquid Chromatography instrument.
Further, above-mentioned ASE-UPLC measures the side of ephedrine hydrochloride in tongxuan lifei pills
Method, described analytical column ACE Excel 2 C18-PFP, flow velocity 0.5ml min-1, column temperature
35 DEG C, detecting wavelength 210nm, sample size is 1 μ L；Mobile phase A is acetonitrile, and flow phase
B is 0.1% phosphoric acid solution；Gradient elution program: 0～3.5min, 2%A, 98%B；
3.5～4min, 2%～90%A, 98%～10%B；4～7min, 90%A, 10%B；
2min is balanced under 2%A, 98%B.
Compared with prior art, the ASE method that the present invention provides saves extraction to the utmost
Time, by original more than 48h, shorten to 40min, and it is clean to eliminate loaded down with trivial details extraction
Change step and the process volatilized, decrease ephedrine hydrochloride in the degraded extracted and in post processing
And loss, it is ensured that the reliability of result.ASE method extracts ephedrine hydrochloride in tongxuan lifei pills
Feasible, it is adaptable to the extraction of ephedrine hydrochloride in tongxuan lifei pills.
Accompanying drawing explanation
Fig. 1 is standard items liquid chromatograms；
Ephedrine hydrochloride high-efficient liquid phase chromatogram in Fig. 2 tongxuan lifei pills.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the claim of the present invention is done the most in detail
Illustrate, but do not constitute any limitation of the invention, any in the claims in the present invention protection
The amendment of the limited number of time that scope is made, still within the claims of the present invention.
Involved in the present invention to percentage composition concentration, in addition to specified otherwise, solute is liquid
Be volumetric concentration, solute is fixing to be mass concentration.
Embodiment 1
1 instrument and reagent
ASE350ASE instrument (Thermo Fisher company of the U.S.)；Agilent 1290 ultra high efficiency
Liquid chromatograph, DAD detector, binary gradient pump, automatic sampler (U.S. Agilent
Company)；XA205DU electronic balance (Mei Tele company of Switzerland)；3K15 supercentrifuge
(Germany Sigma)；Classic UVF Superpure water machine (Britain ELGA).
Ephedrine hydrochloride standard items (National Institute for Food and Drugs Control, lot number 171241-
201007)；Acetonitrile (chromatographically pure, Merck company of Germany), it is pure that remaining reagent is analysis；
2 experimental sections
2.1 sample source
Tongxuan lifei pills (big honeyed bolus, is produced by Guangxi Wuzhou Sanhe Pharmaceutical Co., Ltd,
Lot number 140201,140803,140850,150901,150702).
2.2 standard liquid preparations
Standard reserving solution: accurately weighed ephedrine hydrochloride reference substance 19.77mg, uses hydrochloric acid first
Alcoholic solution (1 → 1000) is settled in 50mL volumetric flask, makes 0.3942g L-1Mark
Quasi-storing solution.
2.3 chromatographic condition
Analytical column ACE Excel 2C18-PFP (2.1mm × 75mm, 2 μm), flow velocity
0.5ml·min-1, column temperature 35 DEG C, detect wavelength 210nm, sample size is 1 μ L.Flowing
Phase A is acetonitrile, and Mobile phase B is 0.1% phosphoric acid solution；Gradient elution program: 0～
3.5min, 2%A, 98%B；3.5～4min, 2%～90%A, 98%～10%B；4～
7min, 90%A, 10%B；2min is balanced under 2%A, 98%B.
2.4 experimental technique
ASE method: accurately weigh sample 1g and be placed in 10mL abstraction pool, with n-hexane pair
Sample carries out except ester that (Extracting temperature is 80 DEG C, and static extraction time is 5min, extraction time
Be 1 time, flush volume 100%) after with methyl alcohol as Extraction solvent, Extracting temperature is 80 DEG C,
Static extraction time is 8min, and extraction time is 3 times.Extraction complete after by extract constant volume
To 25mL, draw 1.5mL in equipped with in the 2mL centrifuge tube of 300mg PSA, whirlpool
2min, 15000r/min are centrifuged 3min, take supernatant and carry out ultra high efficiency liquid phase analysis.
3 results and discussion
The selection of 3.1 liquid phase chromatogram conditions
" Chinese Pharmacopoeia " one uses 0.02mol L-1Potassium dihydrogen phosphate is (containing 0.2% 3
Ethamine, phosphoric acid regulation PH to 2.7) as aqueous phase flow phase, it is contemplated that use buffer salt with
And the inconvenience of regulation flowing phase acidity, attempt flowing phase as aqueous phase with 0.1% phosphoric acid, distinguish
Employing Phenomenex synergi Polar-RP 80A (4.6mm × 250mm, 4 μm),
Agilent ZORBAX SB C18 (4.6mm × 250mm, 5 μm), Thermo
Accucore C18 (2.1mm × 50mm, 2.6 μm), ACE Excel 2C18-PFP
(2.1mm × 75mm, 2 μm) test, and find ACE Excel 2C18-PFP
(2.1mm × 75mm, 2 μm) separating effect is best, chromatographic peak profile is preferable, therefore selects
ACE Excel 2C18-PFP (2.1mm × 75mm, 2 μm) is analytical column, and result is shown in
Fig. 1.
3.2 single factor exploration
Take lot number be 150702 as investigate samples, affect ASE efficiency because have extraction
Solvent, Extracting temperature, extraction time, extraction time etc..These factors have been investigated in this experiment
On the impact of ephedrine hydrochloride extraction efficiency in tongxuan lifei pills, and use orthogonal experiment to carrying
The condition of taking is optimized, and when investigating certain single factor test, only changes the condition of this factor, its
His condition is constant.The investigation of extracting parameter all measures content for commenting with ephedrine hydrochloride HPLC
Valency index.
3.2.1 Extraction solvent and the selection of sampling amount: accurately weigh tongxuan lifei pills sample 2g,
Respectively by n-butanol, ethyl acetate, ammoniacal liquor-n-butanol, ammoniacal liquor-ethyl acetate, ammoniacal liquor-second
Alcohol-ethyl acetate (3:10:90), 1.44% phosphoric acid, alkaline methanol (pH8～9), methyl alcohol
As Extraction solvent, at 100 DEG C, extract 5min, extract 3 times, investigate difference and extract molten
The agent impact on ephedrine hydrochloride extraction effect.
Phosphoric acid or alkaline methanol extraction efficiency are higher, but matrix impact is bigger；Ammonia water-ethanol-
Under the conditions of ethyl acetate (3:10:90), extraction efficiency is higher and matrix impact is less, but considers
Acid, the impact on ASE instrument of the alkali solvent, therefore select methyl alcohol as Extraction solvent.
The 10mL abstraction pool solvent washing finite volume used due to experiment, for 2g sample
Product extract can be insufficient, and therefore selecting sampling amount is 1g.
3.2.2 the selection of Extracting temperature: accurately weigh tongxuan lifei pills sample 1g, use methyl alcohol
As Extraction solvent, 80 DEG C, 100 DEG C, extract respectively 3 times at 120 DEG C, each 8min,
Investigate the different Extracting temperature impact on ephedrine hydrochloride extraction effect.80 DEG C as a result,
100 DEG C, recovery rate obtained by ASE method is on the low side compared with pharmacopeia extracting method at 120 DEG C, can
Can be heated degradable by ephedrine hydrochloride, it is considered to reduce temperature to improve extraction efficiency.
Owing to the boiling point of methyl alcohol is about 64 DEG C, in conjunction with the high pressure penetrability of ASE, therefore select
Extracting method is groped by 70 DEG C, 80 DEG C and 90 DEG C, investigates Extracting temperature to Tongxuanlifei
The extraction efficiency impact of ephedrine hydrochloride in ball.Accurately weigh tongxuan lifei pills 1g, use methyl alcohol
As Extraction solvent, extract respectively at 70 DEG C, 80 DEG C and 90 DEG C 3 times, each 8min,
Investigate the different Extracting temperature impact on ephedrine hydrochloride extraction effect.The results are shown in Table 1.
The different Extracting temperature extraction effect to ephedrine hydrochloride of table 1
From data above, temperature is relatively big on the impact of extraction efficiency, is considering that salt is tingle
During the extraction efficiency of yellow alkali, the impact of its high temperature degradation and used solvent thereof should be taken into full account
Molten boiling point.Extraction efficiency is also had a certain impact by the time, and the time is too short, cannot not extract completely
Entirely, overlong time is then time-consuming, is unfavorable for improving efficiency.To sum up, molten according to the extraction selected
Agent methyl alcohol can determine that temperature at about 80 DEG C, optimize further Extracting temperature and extraction time,
The factors such as cycle-index, impurity purification, seek preferred plan.
3.3ASE extracts Orthogonal experiment results: according to the result of above single factor experiment, really
Determining methyl alcohol is Extraction solvent, uses L9(34) orthogonal test, with Extracting temperature/DEG C (A),
Extraction time/min (B) and these 3 factors of extraction time/time (C) are in tongxuan lifei pills
Ephedrine hydrochloride extracts the impact of content, three levels of each factor, carries out ASE method extraction
The condition optimizing of ephedrine hydrochloride in tongxuan lifei pills.Orthogonal experiments is shown in Table 2, variance
Analysis result is shown in Table 3.
Table 2L9(34) orthogonal test table and interpretation of result
Table 3 analysis of variance table
From orthogonal experiments, affect ephedrine hydrochloride ASE in tongxuan lifei pills and extract
Each factor primary and secondary order of effect is: C (extraction time) > B (extraction time) > A (Extracting temperature),
Obtaining optimum extraction condition is: A2B2C2, i.e. sample weighting amount is 1g, methyl alcohol as Extraction solvent,
Extracting temperature is 80 DEG C, and extraction time is 8min, extraction time 3 times.
3.4 method for cleaning impurity: owing to sample tongxuan lifei pills is big honeyed bolus, make with methyl alcohol
For Extraction solvent, in lactone component that in prescription, polarity is little and pill, carbohydrate impurity dissolution is relatively
Many, matrix is relatively big to the interference of ephedrine hydrochloride liquid phase analysis, needs pre-treatment to remove accordingly
Impurity disturbs.
The least polar impurity purification method is investigated: ephedrine hydrochloride in " Chinese Pharmacopoeia "
Employ ether and carry out the removal of liposoluble constituent, owing to ether is not applied for ASE method,
Sample is pre-processed by trial n-hexane, and Extracting temperature is 80 DEG C, static extraction time
For 5min, extraction time is 1 time, flush volume 100%, found that the little polarity of part
Lipid material is removed, and ephedrine hydrochloride does not the most lose.
3.4.2 carbohydrate method for cleaning impurity is investigated: attempt a certain amount of in abstraction pool underfill
Scavenging material, such as silica gel, neutral alumina, alkali alumina, C18, PSA (N-third
Base ethylenediamine) etc., direct purification sample during extracting.Found that silica gel,
C18 clean-up effect is poor, neutral alumina, alkali alumina clean-up effect preferable, with
The increase of aluminum oxide, clean-up effect is the best, but neutral alumina and alkali alumina are to mesh
Mark compound has certain suction-operated to ephedrine hydrochloride, and loss late is about 15%～18%.
PSA (N-propyl group ethylenediamine) absorption glucide effect is preferable, and does not the most lose,
But relatively big in view of the amount directly adding PSA in abstraction pool, relatively costly, therefore use instead
Quechers purification method.After i.e. ASE extract being settled to 25mL, draw 1.5mL
In equipped with in the 2mL centrifuge tube of a certain amount of PSA, whirlpool 2min, 15000r/min are centrifugal
3min, takes supernatant and carries out ultra high efficiency liquid phase analysis.
3.4.3 purge amount is investigated: draws 1.5mLASE extract respectively and is placed in equipped with 50,
The 2mL of 100,200,300,400,500mgPSA purifies in pipe, whirlpool 2min,
15000r/min takes supernatant after being centrifuged 3min and is analyzed.Found that 300mgPSA
Clean-up effect is best, therefore determines that the purge amount of PSA is 300mg.
3.5 methodological study
3.5.1 linear relationship precision draws 0.3942g L-1Standard reserving solution 1mL, use
Methanol hydrochloride solution (1 → 1000) is settled in 25mL volumetric flask, makes
0.0158g·L-1Standard liquid.Sample size is respectively 0.2,0.4,0.6,0.8,1,1.2
μ L, parallel determination 2 times, with peak area (Y), mass concentration mg (X) is carried out linear regression,
At 0.00315～0.0189g L-1In the range of linearity, linear equation is:
Y=4184.2X+0.3465, linearly dependent coefficient R2=0.9998.
3.5.2 method repeatability and the rate of recovery investigate: accurately weigh tongxuan lifei pills (lot number:
150702) 1g totally 6 parts, more accurately weigh tongxuan lifei pills (lot number: 150702) 0.5g
Totally 6 parts, accurately add ephedrine hydrochloride standard liquid 0.3mL (hydrochloric ephedrine
0.11826mg), extracted by 2.5.1 method and detected.Result such as table 4, repeatability
RSD is 3.0%, and recovery of standard addition scope is 92%～102%, owing to mark-on mode is will
Comparison liquid be equipped with in the small beaker of sample, mixing and diatomite fully dispersed after refill
Entering in abstraction pool, whole transfer process may have certain loss to addition.
Table 4 repeatability and determination of recovery rates
3.6 carry out the instrument repeatability investigation to extracting method with 2 identical ASE instruments
And the comparison of ASE method and official method: take 5 batch sample of tongxuan lifei pills respectively,
Each batch takes 3 parts respectively, carries out instrument 1 and the process of instrument 2 by 2.5.1ASE method；
Taking 5 batch sample of tongxuan lifei pills, each batch takes 2 parts respectively, by 2.5.2 pharmacopeia side
Method processes, and feed liquor is analyzed mutually respectively.Result such as table 5.
Table 5 different instrument checking and ASE method compare with official method
In the tongxuan lifei pills that two ASE instruments obtain, Determination of ephedrine hydrochloride RSD is the fewest
In 5%, the favorable reproducibility of instrument.From the interpretation of result of above 5 lot samples, official method
Due to by environment temperature, reflux rate, time, liquid feeding volume, packaging is closely etc. multiple
The impact of factor, extracted with the batch sample same time, and otherness is relatively big, and reappearance is poor.
The ASE method after optimizing is used to extract ephedrine hydrochloride in tongxuan lifei pills, the reappearance of result
Preferably, extracting relatively completely and the relative standard deviation of CP method is within 5%, controllability is strong.
Claims (5)
1. a method for ephedrine hydrochloride during ASE-UPLC measures tongxuan lifei pills, it is special
Levy and be, comprise the steps: successively
1) accurately weigh sample 1g to be placed in 10mL abstraction pool, with n-hexane, sample is entered
Row extracts except ester, and described Extracting temperature is 80 DEG C, and static extraction time is 5min, extracts
Number of times is 1 time, flush volume 100%, then with methyl alcohol as Extraction solvent, Extracting temperature is
80 DEG C, static extraction time is 8min, and extraction time is 3 times；Extraction will be extracted after completing
Liquid is settled to 25mL, draws 1.5mL in equipped with in the 2mL centrifuge tube of 300mg PSA,
Whirlpool 2min, 15000r/min are centrifuged 3min, take supernatant and carry out ultra high efficiency liquid phase analysis；
2) accurate absorption 0.3942g L-11mL, use volume ratio 1:1000 hydrochloric acid
It is settled in 25mL volumetric flask with methanol solution, makes 0.0158g L-1Standard liquid,
Sample size is respectively 0.2,0.4,0.6,0.8,1,1.2 μ L, and parallel determination 2 times, with peak
Area carries out linear regression to mass concentration mg, at 0.00315～0.0189g L-1Linearly
In the range of, linear equation is: Y=4184.2X+0.3465, linearly dependent coefficient R2=0.9998.
It is tingle that ASE-UPLC the most according to claim 1 measures salt in tongxuan lifei pills
The method of yellow alkali, it is characterised in that described abstraction instrument is ASE350.
It is tingle that ASE-UPLC the most according to claim 1 measures salt in tongxuan lifei pills
The method of yellow alkali, it is characterised in that described Ultra Performance Liquid Chromatography instrument is Agilent 1290
Ultra Performance Liquid Chromatography instrument.
It is tingle that ASE-UPLC the most according to claim 1 measures salt in tongxuan lifei pills
The method of yellow alkali, it is characterised in that described analytical column ACE Excel 2C18-PFP, stream
Speed 0.5ml min-1, column temperature 35 DEG C, detect wavelength 210nm, sample size is 1 μ L；Stream
Dynamic phase A is acetonitrile, and Mobile phase B is 0.1% phosphoric acid solution；Gradient elution program: 0～
3.5min, 2%A, 98%B；3.5～4min, 2%～90%A, 98%～10%B；4～
7min, 90%A, 10%B；2min is balanced under 2%A, 98%B.
It is tingle that ASE-UPLC the most according to claim 1 measures salt in tongxuan lifei pills
The method of yellow alkali, it is characterised in that the preparation method of described standard reserving solution is accurate title
Determining ephedrine hydrochloride reference substance 19.77mg, hydrochloric acid and methyl alcohol by volume ratio 1:1000 are molten
Liquid is settled in 50mL volumetric flask, makes 0.3942g L-1Standard reserving solution.
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| CN107014926A (en) * | 2017-04-20 | 2017-08-04 | 广西壮族自治区梧州食品药品检验所 | The method that the Accelerate solvent extraction joint QuEChERS methods of purification determine ephedrine hydrochloride in reason lung ball |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107014926A (en) * | 2017-04-20 | 2017-08-04 | 广西壮族自治区梧州食品药品检验所 | The method that the Accelerate solvent extraction joint QuEChERS methods of purification determine ephedrine hydrochloride in reason lung ball |
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