CN106950292A - A kind of lung-clearing anti-inflammatory ball quality standard detecting method - Google Patents
A kind of lung-clearing anti-inflammatory ball quality standard detecting method Download PDFInfo
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Abstract
The invention provides a kind of lung-clearing anti-inflammatory ball quality standard detecting method, belong to technical field of traditional Chinese medicines, the preparation of (1) control sample solution；(2) preparation of test sample solution；(3) preparation of negative sample solution；(4) accurate test sample solution, reference substance solution and the negative sample solution injection high performance liquid chromatograph drawn is measured respectively, is produced.The present invention simplifies extraction step, detection method precision is improved, and the content detection control method of the water-bindered pill of lung-clearing anti-inflammatory ball and water-honeyed pill is unified, the water-bindered pill that the method can not only be applied to lung-clearing anti-inflammatory ball is also applied for water-honeyed pill, detection to get up more facilitate, fast.
Description
Technical field
The present invention relates to technical field of traditional Chinese medicines is belonged to, specifically a kind of lung-clearing anti-inflammatory ball quality standard detecting method.
Background technology
Lung-clearing anti-inflammatory ball is a kind of traditional Chinese medicine preparation, and it is by Chinese ephedra, gypsum, earthworm, great burdock achene, lepidium seed, people
Work cow-bezoar, semen armeniacae amarae (stir-fry), antelope's horn composition.It is mainly used in clearing lung and eliminating phlegm, it is relieving cough and asthma.For pulmonary retention of phlegmopyrexia, cough and asthma,
Distending pain in the chest and hypochondrium, yellow thick, the acute attack of the infection of the upper respiratory tract, acute bronchitis and chronic bronchitis of spitting, and lung
Cough phlegm caused by infection is thick, the illness such as out of breath of panting.
The water-bindered pill of lung-clearing anti-inflammatory ball is the medicine that Tianjin Zhongxin Pharmaceutical Group Co produces,
Its quality standard is recorded in State Food and Drug Administration standard YBZ00662010.Under primary standard Chinese ephedra assay
Assay method be high performance liquid chromatography, this method using distillating method extraction, complex steps, cycle are long, and process is bad
Control；And only determine ephedrine hydrochloride content,《Chinese Pharmacopoeia》Herba Ephedrae is to ephedrine hydrochloride and the pseudo- fiber crops of hydrochloric acid
The total amount of yellow alkali is controlled.
The water-honeyed pill of lung-clearing anti-inflammatory ball is the medicine that Tianjin Zhongxin Pharmaceutical Group Co produces
Product, its quality standard record in《Chinese Pharmacopoeia》Version in 2015.Assay method under primary standard Chinese ephedra assay is thin layer
Scanning method, this method extraction step is cumbersome, cycle length, detection method precision are low, and only determines the content of ephedrine hydrochloride,
《Chinese Pharmacopoeia》Total amount of the Herba Ephedrae to ephedrine hydrochloride and pseudoephedrine hydrochloride is controlled.
In order to simplify extraction step, detection method precision is improved, and by the content of the lung-clearing anti-inflammatory ball water-bindered pill and water-honeyed pill
Detection control method is unified, and Tianjin Zhongxin Pharmaceutical Group Co, which conducts a research, has formulated side
Method, the water-bindered pill that the method can not only be applied to lung-clearing anti-inflammatory ball is also applied for water-honeyed pill, and detection to get up more facilitate, fast.
The content of the invention
In view of this, the present invention is intended to provide a kind of lung-clearing anti-inflammatory ball quality standard detecting method.
To reach above-mentioned purpose, the technical proposal of the invention is realized in this way：A kind of lung-clearing anti-inflammatory ball quality standard inspection
Survey method, comprises the following steps：
(1) preparation of control sample solution：Take ephedrine hydrochloride, pseudoephedrine hydrochloride reference substance appropriate, it is accurately weighed, plus
Each 40 μ g of the hydrochloric ephedrines of every 1mL, pseudoephedrine hydrochloride mixed solution is made in methanol, produces；
(2) preparation of test sample solution：Take sample appropriate, it is finely ground, about 2.0g is taken, accurately weighed, precision adds methanol
25mL, weighed weight is ultrasonically treated, lets cool, then weighed weight, and the weight of less loss is supplied with methanol, is shaken up, filtration, takes continuous filter
Liquid, is produced；
(3) preparation of negative sample solution：The ingredients except Chinese ephedra is weighed by prescription, sample is made by formulation and technology,
According still further to the preparation method of the step (2) test sample solution, negative sample solution is made；
(4) it is accurate respectively to draw test sample solution, reference substance solution and negative sample solution injection high performance liquid chromatography
Instrument is measured, and is produced.
Further, the chromatographic condition of the step (4) is as follows：
Chromatographic column：Phenomenex Luna C18,250mm × 4.6mm, 5 μm；
Mobile phase：Acetonitrile -0.02mol/L potassium dihydrogen phosphates, both volume ratios are 4：96；
Column temperature：40℃；
Flow velocity：1.0mL/min；
Detection wavelength：210nm；
Number of theoretical plate is calculated by ephedrine hydrochloride peak should be not less than 8000.
Further, the sample in the step (4) is the water-bindered pill or water-honeyed pill of lung-clearing anti-inflammatory ball.
Further, the solution of injection high performance liquid chromatography is 5~10uL in the step (4).
Further, 0.2% triethylamine is contained in the mobile phase 0.02mol/L potassium dihydrogen phosphates, is adjusted with phosphoric acid
To pH2.7.
Further, the every 1g of the sample is containing Chinese ephedra in terms of the total amount of ephedrine hydrochloride and pseudoephedrine hydrochloride, and the water-bindered pill is not
0.56mg must be less than, water-honeyed pill must not be less than 0.34mg.
Relative to prior art, the present invention has the advantage that：
(1) complex chemical composition in the present invention, realizes efficiently separating for ephedrine hydrochloride and pseudoephedrine hydrochloride, and have
Effect eliminates the interference of other impurities, good stability, precision height, favorable reproducibility, convenient and be easy to grasp.
(2) present invention has reformulated the content limit of this product for " per 1g containing Chinese ephedra with ephedrine hydrochloride and the pseudo- fiber crops of hydrochloric acid
The total amount meter of yellow alkali, the water-bindered pill must not be less than 0.56mg, and water-honeyed pill must not be less than 0.34mg ".
(3) present invention simplifies extraction step, improves detection method precision, and by the water-bindered pill and water-honeyed pill of lung-clearing anti-inflammatory ball
Content detection control method unified, the method can not only be applied to lung-clearing anti-inflammatory ball the water-bindered pill be also applied for water honey
Ball, detection to get up more facilitate, fast.
Brief description of the drawings
Fig. 1 is lung-clearing anti-inflammatory ball (water-bindered pill) reference substance solution chromatogram (Féraud door chromatographic column).
Fig. 2 is lung-clearing anti-inflammatory ball (water-bindered pill) test sample solution chromatogram (Féraud door chromatographic column).
Fig. 3 is lung-clearing anti-inflammatory ball (water-bindered pill) negative sample solution chromatogram (Féraud door chromatographic column).
Fig. 4 is lung-clearing anti-inflammatory ball (water-bindered pill) reference substance solution chromatogram (enlightening horse chromatographic column).
Fig. 5 is lung-clearing anti-inflammatory ball (water-bindered pill) need testing solution chromatogram (enlightening horse chromatographic column).
Fig. 6 is lung-clearing anti-inflammatory ball (water-bindered pill) reference substance solution chromatogram (Shiseido chromatographic column).
Fig. 7 is lung-clearing anti-inflammatory ball (water-bindered pill) need testing solution chromatogram (Shiseido chromatographic column).
Fig. 8 is lung-clearing anti-inflammatory ball (water-honeyed pill) reference substance solution chromatogram (Féraud door chromatographic column).
Fig. 9 is lung-clearing anti-inflammatory ball (water-honeyed pill) test sample solution chromatogram (Féraud door chromatographic column).
Figure 10 is lung-clearing anti-inflammatory ball (water-honeyed pill) negative sample solution chromatogram (Féraud door chromatographic column).
Figure 11 is lung-clearing anti-inflammatory ball (water-honeyed pill) reference substance solution chromatogram (enlightening horse chromatographic column).
Figure 12 is lung-clearing anti-inflammatory ball (water-honeyed pill) need testing solution chromatogram (enlightening horse chromatographic column).
Figure 13 is lung-clearing anti-inflammatory ball (water-honeyed pill) reference substance solution chromatogram (Shiseido chromatographic column).
Figure 14 is lung-clearing anti-inflammatory ball (water-honeyed pill) need testing solution chromatogram (Shiseido chromatographic column).
Embodiment
Embodiment one lung-clearing anti-inflammatory ball (water-bindered pill) quality standard detecting method
1.1 instruments and reagent
Instrument：The high performance liquid chromatographs of Agilent 1200.
Reagent：Acetonitrile (chromatographically pure, Merck companies), methanol (chromatographically pure, Tianjin Concord Technology Co., Ltd.), phosphorus
Acid (analysis is pure, and Tianjin, which is won, reaches your dilute chemical reagent factory), (analysis is pure, and Tianjin, which is won, reaches your dilute chemical reagent for potassium dihydrogen phosphate
Factory), triethylamine (analyzes pure, Tianjin Concord Technology Co., Ltd.), and (analysis is pure, and Tianjin is won up to your dilute chemistry examination for ammoniacal liquor
Agent factory), water is deionized water.
Reference substance：(National Institute for Food and Drugs Control purchases ephedrine hydrochloride, lot number：171241-201007, for containing
Fixed use is measured, purity is that 99.7%), (National Institute for Food and Drugs Control purchases pseudoephedrine hydrochloride, lot number：171237-
201208, for assay, 99.9%) purity be.
Sample (water-bindered pill)：Tianjin Zhongxin Pharmaceutical Group Co's (lot number： 9008789、
9008790、9008791、9008877、9008878、9008879)。
The preparation of 1.2 control sample solution：Take ephedrine hydrochloride, pseudoephedrine hydrochloride reference substance appropriate, it is accurately weighed, plus
The hydrochloric μ g of ephedrine 40.96 of every 1mL, each 41.44 μ g of pseudoephedrine hydrochloride mixed solution is made in methanol, and sample introduction is determined,
Produce, peak sequence is followed successively by：Ephedrine hydrochloride, pseudoephedrine hydrochloride, are as a result shown in Fig. 1.
The preparation of 1.3 test sample solution：Same lot number (9008789) appropriate sample is taken, it is finely ground, about 2.0g is taken, it is accurate
Weighed, precision adds methanol 25mL, and weighed weight, ultrasonically treated 45min (power 500W, frequency 40kHz) lets cool, then weighed
Weight, the weight of less loss is supplied with methanol, is shaken up, and is filtered with 0.45 μm of miillpore filter, takes subsequent filtrate, and sample introduction is determined, produced,
Peak sequence is followed successively by：Ephedrine hydrochloride, pseudoephedrine hydrochloride, are as a result shown in Fig. 2.
1.3.1 the determination of extracting mode
(1) ultrasonic extraction：Same lot number (9008789) appropriate sample is taken, it is finely ground, 2.0g is taken, accurately weighed, precision is added
Methanol 25mL, weighed weight, ultrasonically treated 45min (power 500W, frequency 40kHz) lets cool, then weighed weight, is mended with methanol
The weight of sufficient less loss, shakes up, and is filtered with 0.45 μm of miillpore filter, takes subsequent filtrate, and sample introduction determines, produces, the results are shown in Table 1-1.
(2) refluxing extraction：Same lot number (9008789) appropriate sample is taken, it is finely ground, 2.0g is taken, accurately weighed, precision is added
Methanol 25mL, weighed weight is put and 45min is heated to reflux in water-bath, lets cool, then weighed weight, plus methanol supplies the weight of less loss,
Shake up, filtered with 0.45 μm of miillpore filter, take subsequent filtrate, sample introduction determines, produces, the results are shown in Table 1-1.
The comparison of table 1-1 extracting modes
Conclusion：Using ultrasonic extraction and heating and refluxing extraction mode, ephedrine hydrochloride and hydrochloric acid False path in sample are measured
The total amount difference of alkali is little, it is contemplated that ultrasonic extracting method is simple, therefore uses ultrasonic extraction.
1.3.2 the investigation of extraction time
Same lot number (9008789) appropriate sample is taken, it is finely ground, 2.0g is taken, it is accurately weighed, it is accurate respectively to add methanol
25mL, weighed weight, ultrasonic extraction 15,30,45,60,90min (power 500W, frequency 40kHz), let cool respectively, then weighed
Weight, the weight of less loss is supplied with methanol, is shaken up, and is filtered with 0.45 μm of miillpore filter, takes subsequent filtrate, and sample introduction is determined, produced,
It the results are shown in Table 1-2.
The comparison of table 1-2 extraction times
Conclusion：After ultrasonic extraction 45min, the total amount of ephedrine hydrochloride and pseudoephedrine hydrochloride is basically unchanged in sample,
Therefore the selective extraction time is 45min.
1.3.3 the selection of Extraction solvent
Same lot number (9008789) appropriate sample is taken, it is finely ground, 2.0g is taken, it is accurately weighed, the accurate addition methanol of difference,
70% methanol, 50% methanol, water, each 25mL of ethanol, weighed weight, difference ultrasonic extraction 45min (power 500W, frequency
40kHz), let cool, then weighed weight, the weight of less loss is supplied with respective solvent respectively, is shaken up, is filtered with 0.45 μm of miillpore filter
Cross, take subsequent filtrate, sample introduction determines, produces, the results are shown in Table 1-3.
The comparison of table 1-3 Extraction solvents
Conclusion：Calculate sample in ephedrine hydrochloride and pseudoephedrine hydrochloride total amount, as a result with methanol, 70% methanol and
50% is basically identical as the total amount of solvent extraction；Meanwhile, impurity is less in methanol extract liquid test sample chromatogram, therefore selection first
Alcohol is Extraction solvent.
1.3.4 the investigation of Extraction solvent amount
Same lot number (9008789) appropriate sample is taken, it is finely ground, 2.0g is taken, it is accurately weighed, it is accurate respectively to add methanol
15mL, 25mL, 50mL and 100mL, weighed weight, ultrasonic extraction 45min (power 500W, frequency 40kHz) are let cool, then weighed
Weight, the weight of less loss is supplied with methanol, is shaken up, and is filtered with 0.45 μm of miillpore filter, takes subsequent filtrate, and sample introduction is determined, produced,
It the results are shown in Table 1-4.
The comparison of table 1-4 Extraction solvent amounts
Conclusion：The total amount that Extraction solvent amount is measured when being 15mL is relatively low, later with the increase of Extraction solvent amount, measures salt
The total amount of sour ephedrine and pseudoephedrine hydrochloride does not have significant difference, therefore Extraction solvent amount is defined as 25mL.
The preparation of 1.4 negative sample solution：The ingredients except Chinese ephedra is weighed by prescription, sample is made by formulation and technology,
According still further to the preparation method of 1.3 test sample solution, negative sample solution is made, sample introduction is determined, produced, peak sequence is successively
For：Ephedrine hydrochloride, pseudoephedrine hydrochloride, are as a result shown in Fig. 3.
1.5 chromatographic conditions
Chromatographic column：Phenomenex Luna C18,250mm × 4.6mm, 5 μm；
Mobile phase：Acetonitrile -0.02mol/L potassium dihydrogen phosphates, both volume ratios are 4：96；
Column temperature：40℃；
Flow velocity：1.0mL/min；
Detection wavelength：210nm；
Number of theoretical plate is calculated by ephedrine hydrochloride peak should be not less than 8000.
1.5.1 the selection of mobile phase
Be measured using the chromatographic condition under 1.5, in sample ephedrine hydrochloride and pseudoephedrine hydrochloride chromatographic peak with
Impurity peaks separation is preferable, and peak sequence is followed successively by：Ephedrine hydrochloride, pseudoephedrine hydrochloride, are shown in Fig. 1-2.
1.5.2 the comparison of different chromatographic columns
The chromatographic column (Féraud door, Shiseido, enlightening horse) of three manufacturer productions, using the mobile phase under 1.5, sample separation
Effect is preferable, and peak sequence is followed successively by：Ephedrine hydrochloride, pseudoephedrine hydrochloride, are shown in Fig. 1,2,4,5,6,7.
The preparation of 1.6 standard curves
1.6.1 ephedrine hydrochloride standard curve
Take ephedrine hydrochloride reference substance appropriate, it is accurately weighed, plus methanol be made concentration be per 1mL in hydrochloric Chinese ephedra respectively
The μ g of alkali 10.1345,20.2690,30.4035,40.5380,81.0760,121.6141 reference substance solution, it is accurate respectively to inhale
5 μ L are taken, liquid chromatograph is injected, is analyzed according to 1.5 chromatographic conditions, respective peak area is determined respectively, with the amount of reference substance sample introduction
(μ g) is abscissa, and peak area value is ordinate, tries to achieve regression equation, the results are shown in Table 1-5
Table 1-5 ephedrine hydrochloride standard curves
Conclusion：Ephedrine hydrochloride regression equation is tried to achieve for Y=2160.6X+1.5568, r=0.9999, as a result shows hydrochloric acid
Ephedrine is linear good in 0.050675~0.608100 μ g ranges.
1.6.2 pseudoephedrine hydrochloride standard curve：
Take pseudoephedrine hydrochloride reference substance appropriate, it is accurately weighed, plus methanol be made concentration be per 1mL in hydrochloric puppet respectively
The μ g of ephedrine 10.3047,20.6094,30.9141,41.2187,82.4375,123.6562 reference substance solution, it is smart respectively
5 μ L of close absorption, inject liquid chromatograph, are analyzed according to 1.5 chromatographic conditions, respective peak area are determined respectively, with reference substance sample introduction
Amount (μ g) be abscissa, peak area value is ordinate, tries to achieve regression equation, the results are shown in Table 1-6.
Table 1-6 pseudoephedrine hydrochloride standard curves
Conclusion：Pseudoephedrine hydrochloride regression equation is tried to achieve for Y=2182.7X+1.1705, r=0.9999, as a result shows salt
Sour pseudoephedrine is linear good in 0.051525~0.618300 μ g ranges.
1.6.3 sample introduction replica test
Take same lot number (9008789) appropriate, it is finely ground, 2.0g is taken, accurately weighed, precision adds methanol 25mL, according to 1.3
Test sample solution preparation manipulation, is analyzed, continuous sample introduction 6 times according to 1.5 chromatographic conditions, determines ephedrine hydrochloride and the pseudo- fiber crops of hydrochloric acid
Yellow alkali peak area, the results are shown in Table 1-7.
Table 1-7 sample introduction replica tests
Conclusion：Ephedrine hydrochloride and pseudoephedrine hydrochloride peak area average value are respectively 515,357, RSD difference in sample
For 0.44%, 0.29%, meet the requirements.
1.6.4 reappearance test
Same lot number (9008789) appropriate sample is taken, it is finely ground, 2.0g is taken, it is accurately weighed, it is totally 6 parts, accurate respectively to add first
Alcohol 25mL, according to 1.3 test sample solution preparation manipulations, analyzes according to 1.5 chromatographic conditions, determines, the results are shown in Table 1-8.
Table 1-8 reappearance tests
Conclusion：The average value difference 0.6047 of ephedrine hydrochloride in sample, pseudoephedrine hydrochloride and both total amounts,
0.4143rd, 1.0190mg/g, RSD are respectively 0.44%, 0.39%, 0.36%, are met the requirements.
1.6.5 stability test
Same lot number (9008789) appropriate sample is taken, it is finely ground, 2.0g is taken, accurately weighed, precision adds methanol 25mL, presses
According to 1.3 test sample solution preparation manipulations, according to 1.5 chromatographic conditions respectively 0,4,8,12,18,24h sample introductions, determine, as a result
It is shown in Table 1-9.
Table 1-9 stability tests
Conclusion：Ephedrine hydrochloride and pseudoephedrine hydrochloride peak area average value are respectively 518,359, RSD difference in sample
For 0.29%, 0.46%, meet the requirements.
1.6.6 recovery test
Same lot number (9008789) appropriate sample is taken, it is finely ground, 1.0g is taken, accurately weighed, totally 6 parts, accurate addition respectively contains
There is the methanol mixed reference substance solution that ephedrine hydrochloride, Pseudo-ephedrine Hydrochloride Concentration are respectively 24.8851,16.7193 μ g/mL
25mL, according to 1.3 test sample solution preparation manipulations, is made for rate of recovery test sample solution, according to 1.5 chromatographic conditions point
Analysis, the results are shown in Table 1-10,1-11.
Table 1-10 ephedrine hydrochloride recovery tests
Table 1-11 pseudoephedrine hydrochloride recovery tests
Conclusion：Calculate the rate of recovery, as a result ephedrine hydrochloride, pseudoephedrine hydrochloride average recovery rate be respectively 100.04%,
100.15%, RSD are respectively 0.50%, 0.52%, as a result meet regulation.
1.7 samples are determined
The sample of 6 different lot numbers is taken, according to 1.3 test sample solution preparation manipulations, is analyzed according to 1.5 chromatographic conditions,
Determine, calculate ephedrine hydrochloride, the content of pseudoephedrine hydrochloride in sample, the results are shown in Table 1-12.
Table 1-12 sample size measurement results
Influence of the 1.8 different chromatographic columns to assay
The test sample solution for taking lot number to be 9008789, is respectively adopted Féraud door phenomenex Luna C18 (2) color
Spectrum post (see Fig. 1-2), enlightening horse Diamonsil-C18 chromatographic columns (see Fig. 1-5), Shiseido CAPCELL PAK-C18 chromatographic columns (see
Fig. 1-7), with the high performance liquid chromatographs of Agilent 1200, analyze, determine according to 1.5 chromatographic conditions, peak sequence is followed successively by：
Ephedrine hydrochloride, pseudoephedrine hydrochloride, calculate the content of ephedrine hydrochloride and pseudoephedrine hydrochloride in sample, the results are shown in Table 1-
13。
Influence of the table 1-13 difference chromatographic columns to assay
Conclusion：As a result show that different chromatographic column assay results are basically identical.
The formulation of 1.9 content limits
Multiple batches of lung-clearing anti-inflammatory ball sample is taken, according to 1.3 test sample solution preparation manipulations, according to 1.5 chromatographic conditions point
Analysis, determines and calculates the content of ephedrine hydrochloride in sample, pseudoephedrine hydrochloride.The Herba Ephedrae content used according to correspondence,
The rate of transform in lung-clearing anti-inflammatory ball (water-bindered pill) actual production process index components is calculated, 1-14 is the results are shown in Table.
Six batches of clearing lung-heat water-bindered pill sample size measurement results of table 1-14
Conclusion：Criticize rate of transform result of calculation to show, in lung-clearing anti-inflammatory ball water-bindered pill production process, ephedrine hydrochloride and hydrochloric acid are pseudo-
The rate of transform of ephedrine total amount is between 63.2%~75.2%, and mean transferred rate is up to 69.4%.The method of the lung-clearing anti-inflammatory ball water-bindered pill
Determine production technology：Eight taste medicinal materials, in addition to calculus bovis factitius, Cornu Saigae Tataricae powder is broken into impalpable powder, and the Six-element such as remaining Chinese ephedra is ground into fine powder,
With antelope's horn and calculus bovis factitius powder facing-up, mix, sieving.With water pill, the water-bindered pill is made, dries, produces.The technological process of production
Mainly include the processes such as pulverizing medicinal materials, mixing, sterilizing, general ball, shaping, drying.According to the observation to actual production process, analysis
Loss and during drying process in sample representation, crushing process when index components rate of transform level is mainly examined with Herba Ephedrae
Between the factor such as longer (55 DEG C of drying temperature, time be more than 72 hours) it is relevant.
According to this product recipe quantity and preparation method, through conversion, this product is per 1g 100mg containing Herba Ephedrae, and this product is theoretical per 1g samples
The total amount of upper hydrochloric ephedrine and pseudoephedrine hydrochloride should be 0.8mg.According to Chinese Pharmacopoeia one Chinese ephedra medicine materical crude slice of version in 2015
The total amount of hydrochloric ephedrine and pseudoephedrine hydrochloride must not be less than 0.80% requirement under, with reference in actual production process
70% rate of transform situation is calculated, and fixes tentatively the content limit of this product for " per 1g containing Chinese ephedra with ephedrine hydrochloride (C10H15NO·
) and pseudoephedrine hydrochloride (C HCl10H15NOHCl total amount meter), must not be less than 0.56mg ".
Embodiment two lung-clearing anti-inflammatory ball (water-honeyed pill) quality standard detecting method
2.1 instruments and reagent
Instrument：The high performance liquid chromatographs of Agilent 1200.
Reagent：Acetonitrile (chromatographically pure, Merck companies), methanol (chromatographically pure, Tianjin Concord Technology Co., Ltd.), phosphorus
Acid (analysis is pure, and Tianjin, which is won, reaches your dilute chemical reagent factory), (analysis is pure, and Tianjin, which is won, reaches your dilute chemical reagent for potassium dihydrogen phosphate
Factory), triethylamine (analyzes pure, Tianjin Concord Technology Co., Ltd.), and (analysis is pure, and Tianjin is won up to your dilute chemistry examination for ammoniacal liquor
Agent factory), water is deionized water.
Reference substance：(National Institute for Food and Drugs Control purchases ephedrine hydrochloride, lot number：171241-201007, for containing
Fixed use is measured, purity is that 99.7%), (National Institute for Food and Drugs Control purchases pseudoephedrine hydrochloride, lot number：171237-
201208, for assay, 99.9%) purity be.
Sample (water-honeyed pill)：Tianjin Zhongxin Pharmaceutical Group Co's (lot number： 9210036、
7870171、7870172、8370001、8370002、8510003、8510004、8510005、 9210060、9210061、
9210062、9210072、9210073、9210074)。
The preparation of 2.2 control sample solution：Take ephedrine hydrochloride, pseudoephedrine hydrochloride reference substance appropriate, it is accurately weighed, plus
The hydrochloric μ g of ephedrine 40.54 of every 1mL, each 41.22 μ g of pseudoephedrine hydrochloride mixed solution is made in methanol, and sample introduction is determined,
Produce, peak sequence is followed successively by：Ephedrine hydrochloride, pseudoephedrine hydrochloride, are as a result shown in Fig. 8.
The preparation of 2.3 test sample solution：Same lot number (9210036) appropriate sample is taken, it is finely ground, about 2.0g is taken, it is accurate
Weighed, precision adds methanol 25mL, and weighed weight, ultrasonically treated 30min (power 500W, frequency 40kHz) lets cool, then weighed
Weight, the weight of less loss is supplied with methanol, is shaken up, and is filtered with 0.45 μm of miillpore filter, takes subsequent filtrate, and sample introduction is determined, produced,
Peak sequence is followed successively by：Ephedrine hydrochloride, pseudoephedrine hydrochloride, are as a result shown in Fig. 9.
2.3.1 the determination of extracting mode
(1) ultrasonic extraction：Same lot number (9210036) appropriate sample is taken, it is finely ground, 2.0g is taken, accurately weighed, precision is added
Methanol 25mL, weighed weight, ultrasonically treated 30min (power 500W, frequency 40kHz) lets cool, then weighed weight, is mended with methanol
The weight of sufficient less loss, shakes up, and is filtered with 0.45 μm of miillpore filter, takes subsequent filtrate, and sample introduction determines, produces, the results are shown in Table 2-1.
(2) refluxing extraction：Same lot number (9210036) appropriate sample is taken, it is finely ground, 2.0g is taken, accurately weighed, precision is added
Methanol 25mL, weighed weight is put and 30min is heated to reflux in water-bath, lets cool, then weighed weight, plus methanol supplies the weight of less loss,
Shake up, filtered with 0.45 μm of miillpore filter, take subsequent filtrate, sample introduction determines, produces, the results are shown in Table 2-1.
The comparison of table 2-1 extracting modes
Conclusion：Using ultrasonic extraction and heating and refluxing extraction mode, ephedrine hydrochloride and hydrochloric acid False path in sample are measured
The total amount difference of alkali is little, it is contemplated that ultrasonic extracting method is simple, therefore uses ultrasonic extraction.
2.3.2 the investigation of extraction time
Same lot number (9210036) appropriate sample is taken, it is finely ground, 2.0g is taken, it is accurately weighed, it is accurate respectively to add methanol
25mL, weighed weight, ultrasonic extraction 15,30,45,60,90min (power 500W, frequency 40kHz), let cool respectively, then weighed
Weight, the weight of less loss is supplied with methanol, is shaken up, and is filtered with 0.45 μm of miillpore filter, takes subsequent filtrate, and sample introduction is determined, produced,
It the results are shown in Table 2-2.
The comparison of table 2-2 extraction times
Conclusion：The total amount highest of ephedrine hydrochloride and pseudoephedrine hydrochloride in ultrasonic extraction 45min, sample, therefore selection
Extraction time is 45min.
2.3.3 the selection of Extraction solvent
Same lot number (9210036) appropriate sample is taken, it is finely ground, 2.0g is taken, it is accurately weighed, it is accurate respectively to add methanol, ammonia
Water-methanol-ethyl acetate (4:10:90), ammoniacal liquor-methanol-ethyl acetate (4:50:50), ammoniacal liquor-methanol-ethyl acetate (4:
80:20) each 25mL, and first with the wetting of 3mL ammoniacal liquor again plus it is accurate add ethyl acetate 25mL, weighed weight, respectively ultrasound carry
30min (power 500W, frequency 40kHz) is taken, is let cool, then weighed weight, the weight of less loss is supplied with respective solvent respectively,
Shake up, filtered with 0.45 μm of miillpore filter, take subsequent filtrate, sample introduction determines, produces, the results are shown in Table 2-3.
The comparison of table 2-3 Extraction solvents
Conclusion：The total amount of ephedrine hydrochloride and pseudoephedrine hydrochloride in sample is calculated, it is as a result preferable using methanol as solvent
Therefore selection methanol is Extraction solvent.
2.3.4 the investigation of Extraction solvent amount
Same lot number (9210036) appropriate sample is taken, it is finely ground, 2.0g is taken, it is accurately weighed, it is accurate respectively to add methanol
25mL, 50mL and 100mL, weighed weight, ultrasonic extraction 30min (power 500W, frequency 40kHz) are let cool, then weighed weight,
The weight of less loss is supplied with methanol, is shaken up, is filtered with 0.45 μm of miillpore filter, subsequent filtrate is taken, sample introduction is determined, produced, as a result
It is shown in Table 2-4.
The comparison of table 2-4 Extraction solvent amounts
Conclusion：With the increase of Extraction solvent amount, the total amount of ephedrine hydrochloride and pseudoephedrine hydrochloride is measured without obvious
Difference, therefore Extraction solvent amount is defined as 25mL.
The preparation of 2.4 negative sample solution：The ingredients except Chinese ephedra is weighed by prescription, sample is made by formulation and technology,
According still further to the preparation method of 2.3 test sample solution, negative sample solution is made, sample introduction is determined, produced, peak sequence is successively
For：Ephedrine hydrochloride, pseudoephedrine hydrochloride, are as a result shown in Figure 10.
2.5 chromatographic conditions
Chromatographic column：Phenomenex Luna C18,250mm × 4.6mm, 5 μm；
Mobile phase：Acetonitrile -0.02mol/L potassium dihydrogen phosphates, both volume ratios are 4：96；
Column temperature：40℃；
Flow velocity：1.0mL/min；
Detection wavelength：210nm；
Number of theoretical plate is calculated by ephedrine hydrochloride peak should be not less than 8000.
2.5.1 the selection of mobile phase
Be measured using the chromatographic condition under 2.5, in sample ephedrine hydrochloride and pseudoephedrine hydrochloride chromatographic peak with
Impurity peaks separation is preferable, and peak sequence is followed successively by：Ephedrine hydrochloride, pseudoephedrine hydrochloride, are shown in Fig. 9.
2.5.2 the comparison of different chromatographic columns
The chromatographic column (Féraud door, Shiseido, enlightening horse) of three manufacturer productions, using the mobile phase under 2.5, sample separation
Effect is preferable, and peak sequence is followed successively by：Ephedrine hydrochloride, pseudoephedrine hydrochloride, are shown in Fig. 8,9,11,12,13,14.
The preparation of 2.6 standard curves
2.6.1 ephedrine hydrochloride standard curve
Take ephedrine hydrochloride reference substance appropriate, it is accurately weighed, plus methanol be made concentration be per 1mL in hydrochloric Chinese ephedra respectively
The μ g of alkali 10.1345,20.2690,30.4035,40.5380,81.0760,121.6141 reference substance solution, it is accurate respectively to inhale
5 μ L are taken, liquid chromatograph is injected, is analyzed according to 2.5 chromatographic conditions, respective peak area is determined respectively, with the amount of reference substance sample introduction
(μ g) is abscissa, and peak area value is ordinate, tries to achieve regression equation, the results are shown in Table 2-5
Table 2-5 ephedrine hydrochloride standard curves
Conclusion：Ephedrine hydrochloride regression equation is tried to achieve for Y=2160.6X+1.5568, r=0.9999, as a result shows hydrochloric acid
Ephedrine is linear good in 0.050675~0.608100 μ g ranges.
2.6.2 pseudoephedrine hydrochloride standard curve：
Take pseudoephedrine hydrochloride reference substance appropriate, it is accurately weighed, plus methanol be made concentration be per 1mL in hydrochloric puppet respectively
The μ g of ephedrine 10.3047,20.6094,30.9141,41.2187,82.4375,123.6562 reference substance solution, it is smart respectively
5 μ L of close absorption, inject liquid chromatograph, are analyzed according to 1.5 chromatographic conditions, respective peak area are determined respectively, with reference substance sample introduction
Amount (μ g) be abscissa, peak area value is ordinate, tries to achieve regression equation, the results are shown in Table 2-6.
Table 2-6 pseudoephedrine hydrochloride standard curves
Conclusion：Pseudoephedrine hydrochloride regression equation is tried to achieve for Y=2182.7X+1.1705, r=0.9999, as a result shows salt
Sour pseudoephedrine is linear good in 0.051525~0.618300 μ g ranges.
2.6.3 sample introduction replica test
Take same lot number (9210036) appropriate, it is finely ground, 2.0g is taken, accurately weighed, precision adds methanol 25mL, according to 2.3
Test sample solution preparation manipulation, is analyzed, continuous sample introduction 6 times according to 2.5 chromatographic conditions, determines ephedrine hydrochloride and the pseudo- fiber crops of hydrochloric acid
Yellow alkali peak area, the results are shown in Table 2-7.
Table 2-7 sample introduction replica tests
Conclusion：Ephedrine hydrochloride and pseudoephedrine hydrochloride peak area average value are respectively 359,331, RSD difference in sample
For 0.38%, 0.82%, meet the requirements.
2.6.4 reappearance test
Same lot number (9210036) appropriate sample is taken, it is finely ground, 2.0g is taken, it is accurately weighed, it is totally 6 parts, accurate respectively to add first
Alcohol 25mL, according to 2.3 test sample solution preparation manipulations, analyzes according to 2.5 chromatographic conditions, determines, the results are shown in Table 2-8.
Table 2-8 reappearance tests
Conclusion：The average value difference 0.4209 of ephedrine hydrochloride in sample, pseudoephedrine hydrochloride and both total amounts,
0.3869th, 0.8078mg/g, RSD are respectively 0.06%, 0.80%, 0.39%, are met the requirements.
2.6.5 stability test
Same lot number (9210036) appropriate sample is taken, it is finely ground, 2.0g is taken, accurately weighed, precision adds methanol 25mL, presses
According to 2.3 test sample solution preparation manipulations, according to 2.5 chromatographic conditions respectively 0,2,4,8,12,24h sample introductions, determine, as a result
It is shown in Table 2-9.
Table 2-9 stability tests
Conclusion：Ephedrine hydrochloride and pseudoephedrine hydrochloride peak area average value are respectively 360,333, RSD difference in sample
For 0.58%, 0.84%, meet the requirements.
2.6.6 recovery test
Same lot number (9210036) appropriate sample is taken, it is finely ground, 1.0g is taken, accurately weighed, totally 6 parts, accurate addition respectively contains
There is the methanol mixed reference substance solution that ephedrine hydrochloride, Pseudo-ephedrine Hydrochloride Concentration are respectively 16.2152,16.4875 μ g/mL
25mL, according to 2.3 test sample solution preparation manipulations, is made for rate of recovery test sample solution, according to 2.5 chromatographic conditions point
Analysis, the results are shown in Table 2-10,2-11.
Table 2-10 ephedrine hydrochloride recovery tests
Table 2-11 pseudoephedrine hydrochloride recovery tests
Conclusion：Calculate the rate of recovery, as a result ephedrine hydrochloride, pseudoephedrine hydrochloride average recovery rate be respectively 97.82%,
98.29%, RSD are respectively 0.57%, 0.64%, as a result meet regulation.
2.7 samples are determined
The sample of 11 different lot numbers is taken, according to 2.3 test sample solution preparation manipulations, analyzes, surveys by 2.5 chromatographic conditions
It is fixed, ephedrine hydrochloride, the content of pseudoephedrine hydrochloride in sample are calculated, 2-12 is the results are shown in Table.
Table 2-12 sample size measurement results
Influence of the 2.8 different chromatographic columns to assay
The test sample solution for taking lot number to be 9210036, is respectively adopted Féraud door phenomenex Luna C18 (2) color
Spectrum post (see Fig. 2-3), enlightening horse Diamonsil-C18 chromatographic columns (see Fig. 2-5), Shiseido CAPCELL PAK-C18 chromatographic columns (see
Fig. 2-7), with the high performance liquid chromatographs of Agilent 1200, analyze, determine according to 2.5 chromatographic conditions, peak sequence is followed successively by：
Ephedrine hydrochloride, pseudoephedrine hydrochloride, calculate the content of ephedrine hydrochloride and pseudoephedrine hydrochloride in sample, the results are shown in Table 2-
13。
Influence of the table 2-13 difference chromatographic columns to assay
Conclusion：As a result show that different chromatographic column assay results are basically identical.
The formulation of 2.9 content limits
Multiple batches of lung-clearing anti-inflammatory ball sample is taken, according to 2.3 test sample solution preparation manipulations, according to 2.5 chromatographic conditions point
Analysis, determines and calculates the content of ephedrine hydrochloride in sample, pseudoephedrine hydrochloride.The Herba Ephedrae content used according to correspondence,
The rate of transform in lung-clearing anti-inflammatory ball (water-honeyed pill) actual production process index components is calculated, 2-14 is the results are shown in Table.
Six batches of clearing lung-heat water-bindered pill sample size measurement results of table 2-14
Conclusion：Rate of transform result of calculation is criticized to show, in lung-clearing anti-inflammatory ball water-honeyed pill production process, ephedrine hydrochloride and hydrochloric acid
The rate of transform of pseudoephedrine total amount is between 62%~89%, and mean transferred rate reaches 72.4%.Lung-clearing anti-inflammatory ball (water-honeyed pill)
Legal production technology be：Eight taste medicinal materials, in addition to calculus bovis factitius, Cornu Saigae Tataricae powder is broken into impalpable powder, and the Six-element such as remaining Chinese ephedra is crushed
Into fine powder, with antelope's horn and calculus bovis factitius powder facing-up, mix, sieving.Add suitable quantity of water system per 60~80g of 100g powder refined honeys
Ball, is made water-honeyed pill, dries, produces.The technological process of production mainly includes pulverizing medicinal materials, mixing, sterilizing, mechanism water-honeyed pill, whole
The processes such as shape, drying.According to the observation to actual production process, analysis indexes composition rate of transform level is mainly examined with Herba Ephedrae
Longer (70-80 DEG C of drying temperature, the time is 36 small loss and drying process time in sample representation, crushing process when testing
When more than) etc. factor it is relevant.
According to this product recipe quantity and preparation method, through conversion, this product is per 1g 60mg containing Herba Ephedrae, and this product is theoretical per 1g samples
The total amount of upper hydrochloric ephedrine and pseudoephedrine hydrochloride should be 0.48mg.According to Chinese Pharmacopoeia one Chinese ephedra medicine materical crude slice of version in 2015
The total amount of hydrochloric ephedrine and pseudoephedrine hydrochloride must not be less than 0.80% requirement under, with reference in actual production process
70% rate of transform situation is calculated, and fixes tentatively the content limit of this product for " per 1g containing Chinese ephedra with ephedrine hydrochloride (C10H15NO·
) and pseudoephedrine hydrochloride (C HCl10H15NOHCl total amount meter), must not be less than 0.34mg ".
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, all essences in the present invention
God is with principle, and any modifications, equivalent substitutions and improvements made etc. should be included within the scope of the present invention.
Claims (6)
1. a kind of lung-clearing anti-inflammatory ball quality standard detecting method, it is characterised in that：Comprise the following steps：
(1) preparation of control sample solution：Take ephedrine hydrochloride, pseudoephedrine hydrochloride reference substance appropriate, it is accurately weighed, plus methanol
Each 40 μ g of the hydrochloric ephedrines of every 1mL, pseudoephedrine hydrochloride mixed solution is made, produces；
(2) preparation of test sample solution：Take sample appropriate, it is finely ground, about 2.0g is taken, accurately weighed, precision adds methanol 25mL,
Weighed weight, it is ultrasonically treated, let cool, then weighed weight, the weight of less loss is supplied with methanol, is shaken up, filters, takes subsequent filtrate, i.e.,
；
(3) preparation of negative sample solution：The ingredients except Chinese ephedra is weighed by prescription, sample is made by formulation and technology, then press
According to the preparation method of the step (2) test sample solution, negative sample solution is made；
(4) accurate test sample solution, reference substance solution and the negative sample solution injection high performance liquid chromatograph drawn enters respectively
Row is determined, and is produced.
2. lung-clearing anti-inflammatory ball quality standard detecting method according to claim 1, it is characterised in that：The step (4)
Chromatographic condition is as follows：
Chromatographic column：Phenomenex Luna C18,250mm × 4.6mm, 5 μm；
Mobile phase：Acetonitrile -0.02mol/L potassium dihydrogen phosphates, both volume ratios are 4：96；
Column temperature：40℃；
Flow velocity：1.0mL/min；
Detection wavelength：210nm；
Number of theoretical plate is calculated by ephedrine hydrochloride peak should be not less than 8000.
3. lung-clearing anti-inflammatory ball quality standard detecting method according to claim 1, it is characterised in that：In the step (2)
Sample be lung-clearing anti-inflammatory ball the water-bindered pill or water-honeyed pill.
4. lung-clearing anti-inflammatory ball quality standard detecting method according to claim 1, it is characterised in that：In the step (4)
The solution for injecting high performance liquid chromatography is 5~10uL.
5. lung-clearing anti-inflammatory ball quality standard detecting method according to claim 2, it is characterised in that：The mobile phase
Contain 0.2% triethylamine in 0.02mol/L potassium dihydrogen phosphates, adjusted with phosphoric acid to pH2.7.
6. lung-clearing anti-inflammatory ball quality standard detecting method according to claim 1, it is characterised in that：The sample contains per 1g
Chinese ephedra is in terms of the total amount of ephedrine hydrochloride and pseudoephedrine hydrochloride, and the water-bindered pill must not be less than 0.56mg, and water-honeyed pill must not be less than
0.34mg。
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