CN107807191A - A kind of method for determining plurality of active ingredients in the own new tablets of clo - Google Patents
A kind of method for determining plurality of active ingredients in the own new tablets of clo Download PDFInfo
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- CN107807191A CN107807191A CN201710885726.1A CN201710885726A CN107807191A CN 107807191 A CN107807191 A CN 107807191A CN 201710885726 A CN201710885726 A CN 201710885726A CN 107807191 A CN107807191 A CN 107807191A
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- clo
- cefaclor
- reference substance
- bromhexine hydrochloride
- new tablets
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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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- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses a kind of method for determining plurality of active ingredients in the own new tablets of clo.This method is using Cefaclor, bromhexine hydrochloride as reference substance, precision draws reference substance solution and need testing solution, inject high performance liquid chromatograph, measure, collection of illustrative plates is recorded, the collection of illustrative plates of reference substance and test sample is produced, obtained collection of illustrative plates is handled, Cefaclor in need testing solution, hydrochloric acid bromine are carried out qualitative and quantitative, and then calculate to obtain Cefaclor, the content of bromhexine hydrochloride in the own new tablets of clo.Each chromatographic peak separation of detection method is preferable, baseline is steady, peak type is good, it is repeated preferable, this method has good linear relationship, precision, stability, the rate of recovery, Cefaclor, bromhexine hydrochloride component content in the own new tablets of clo can be accurately detected, reaches the purpose that the own new tablets of clo are carried out with quality control.
Description
Technical field
The invention belongs to analysis technical field, and in particular to a kind of side for determining plurality of active ingredients in the own new tablets of clo
Method.
Background technology
The own new tablets of clo are the prescription preparation that the honest Qingjian River pharmacy in Jiangsu produces according to China National Drug Standard, mainly
The patient of expectoration is not easy for treating respiratory tract infection caused by sensitive bacteria with sticky sputum.
The preparation method of the own new tablets of clo is：8.77g bromhexine hydrochlorides are taken to be added in suitable decentralized medium, it is stand-by.Again
Appropriate pharmaceutic adjuvant is taken to be mixed with 2000g Cefaclor raw material.It is above-mentioned scattered with containing cephalo gram containing bromhexine hydrochloride
The intermediate of Lip river raw material is sufficiently mixed granulation, by drying, tabletting, film coating, packaging, produces.Wherein mainly contain in product
There are Cefaclor and bromhexine hydrochloride, therefore, oneself new content is controlled to clo, realizes plurality of active ingredients separation inspection
Survey, its quality control is had important practical significance.
The content of the invention
It is an object of the invention to provide a kind of method for determining plurality of active ingredients in the own new tablets of clo, with measure gram
The content of Cefaclor and bromhexine hydrochloride in the own new tablets in Lip river, and then quality control is carried out to the own new tablets of clo.
The present invention is achieved by the following technical solutions：
A kind of method for determining plurality of active ingredients in the own new tablets of clo, comprises the following steps：
The preparation of reference substance solution：Cefaclor reference substance, bromhexine hydrochloride reference substance plus methanol dissolving are weighed, every 1mL is made
Containing μ g of Cefaclor 500, μ g of bromhexine hydrochloride 20, mixed reference substance solution；
The preparation of need testing solution：Take the own new tablets of clo appropriate, add methanol to dissolve, filter and produce；
Chromatographic condition is as follows：
Chromatographic column：Octadecyl silane chromatographic column；Mobile phase：0.005mol/L TBAHs, PH adjust to
3.2 ± 0.1 aqueous solution-methanol=45：55；Flow velocity：0.9mL/min ~1.1mL/min；Detection wavelength：240~245nm；Column temperature：
35℃~45℃；Sample size：8μL ~12μL；
Theoretical cam curve：Calculated with Cefaclor peak and be more than or equal to 2000；
Detection method：Precision draws reference substance solution and need testing solution, injects high performance liquid chromatograph, measure, records collection of illustrative plates,
The collection of illustrative plates of reference substance and test sample is produced, compares Cefaclor, bromhexine hydrochloride equation of linear regression, to head in need testing solution
Spore clo, bromhexine hydrochloride carry out qualitative and quantitative, and then calculate to obtain Cefaclor in the own new tablets of clo, bromhexine hydrochloride
Content.
The Cefaclor equation of linear regression y=2,339,110.2857x-28,344.9333, R 2=1.0000, line
Property is good.
The bromhexine hydrochloride equation of linear regression y=11,440,278.5714 x -35,074.7333, R2=
0.9991, it is linear good.
Further improvement project is the present invention：
The mobile phase is 0.005mol/L TBAHs, and PH is adjusted to 3.2 aqueous solution-methanol=45：55, column temperature is
40 DEG C, Detection wavelength 243nm.
The present invention further improvement project be：
The mobile phase is 0.005mol/L TBAHs, and PH is adjusted to 3.1 aqueous solution-methanol=45：55, column temperature is
35 DEG C, Detection wavelength 240nm.
The present invention further improvement project be：
The mobile phase is 0.005mol/L TBAHs, and PH is adjusted to 3.3 aqueous solution-methanol=45：55, column temperature is
45 DEG C, Detection wavelength 245nm.
Beneficial effects of the present invention are：
Each chromatographic peak separation of detection method is preferable, and baseline is steady, and peak type is good, and preferably, this method has good repeatability
Linear relationship, precision, stability, the rate of recovery, can accurately detect in the own new tablets of clo Cefaclor and hydrochloric acid bromine oneself
New component content, reach the purpose that the own new tablets of clo are carried out with quality control.
Instrument used in the present invention and reagent are as follows：
1st, high performance liquid chromatograph：Waters companies e2695-2998 types.
2nd, reagent：Reference substance Cefaclor, bromhexine hydrochloride are purchased from National Institute for Food and Drugs Control；
The own new tablets of clo：Honest Qingjian River pharmaceutical Co. Ltd self-control.
Brief description of the drawings：Fig. 1 is the reference substance spectrogram and test sample spectrogram of gained under the chromatographic condition of embodiment 1；
Fig. 2 is the reference substance spectrogram and test sample spectrogram of gained under the chromatographic condition of embodiment 2；
Fig. 3 is the reference substance spectrogram and test sample spectrogram of gained under the chromatographic condition of embodiment 3；
Fig. 4 is the gained chromatogram of embodiment 4；
Fig. 5 is Cefaclor peak area value and the linear relationship chart of concentration；
Fig. 6 is bromhexine hydrochloride peak area value and the linear relationship chart of concentration.
Form is described in further details to present disclosure again by the following examples, but not this should not be interpreted as with regard to this
Invent in above-mentioned subject area and be only limitted to following examples.It is general according to this area under the premise of the above-mentioned technology of the present invention is not departed from
The modification of corresponding replacement or change that logical technological know-how and customary means are made, is included in the present invention.
Embodiment 1
The preparation of reference substance solution：Cefaclor reference substance, bromhexine hydrochloride reference substance plus methanol dissolving are weighed, every 1mL is made
Containing μ g of Cefaclor 500, μ g of bromhexine hydrochloride 20, mixed reference substance solution；
The preparation of need testing solution：The own new tablets 0.42g of clo for taking lot number to be 20160421, adds methanol to dissolve, filters and produce
Need testing solution；
Chromatographic condition is as follows：
Chromatographic column：Octadecyl silane chromatographic column；Mobile phase：0.005mol/L TBAHs, PH adjust to
3.2 aqueous solution-methanol=45：55；Flow velocity：1mL/min；Detection wavelength：243nm；Column temperature：40℃；Sample size：10μL；
Theoretical cam curve：Calculated with Cefaclor peak and be more than or equal to 2000；
Detection method：Precision draws reference substance solution and need testing solution, injects high performance liquid chromatograph, measure, records collection of illustrative plates,
As shown in Figure 1.
According to testing result, in the own new tablets of every clo, Cefaclor must not be less than 237.5mg, and bromhexine hydrochloride is not
8.24mg must be less than.
Embodiment 2
The preparation of reference substance solution and need testing solution is the same as embodiment 1.
Chromatographic condition is as follows：
Chromatographic column：Octadecyl silane chromatographic column；Mobile phase：0.005mol/L TBAHs, PH adjust to
3.1 aqueous solution-methanol=45：55；Flow velocity：1mL/min；Detection wavelength：240nm；Column temperature：35℃；Sample size：10μL；
Theoretical cam curve：Calculated with Cefaclor peak and be more than or equal to 2000；
Detection method：Precision draws reference substance solution and need testing solution, injects high performance liquid chromatograph, measure, records collection of illustrative plates,
As shown in Figure 2.
According to testing result, in the own new tablets of every clo, Cefaclor must not be less than 237.5mg, and bromhexine hydrochloride is not
8.24mg must be less than.
Embodiment 3
The preparation of reference substance solution and need testing solution is the same as embodiment 1.
Chromatographic condition is as follows：
Chromatographic column：Octadecyl silane chromatographic column；Mobile phase：0.005mol/L TBAHs, PH adjust to
3.3 aqueous solution-methanol=45：55；Flow velocity：1.1mL/min；Detection wavelength：246nm
Column temperature：45℃；Sample size：10μL；
Theoretical cam curve：Calculated with Cefaclor peak and be more than or equal to 2000；
Detection method：Precision draws reference substance solution and need testing solution, injects high performance liquid chromatograph, measure, records collection of illustrative plates,
As shown in Figure 2.
According to testing result, in the own new tablets of every bag of clo, Cefaclor must not be less than 237.5mg, and bromhexine hydrochloride is not
8.24mg must be less than.
Embodiment 4：Interference test
The preparation of reference substance solution is the same as embodiment 1.
The preparation of full auxiliary material solution：1 gram of starch, 0.02g adhesives are taken, adds methanol constant volume to be shaken up, filtering is to 500ml
；Chromatographic condition is the same as embodiment 1.
Detection method：Precision draws reference substance solution, full auxiliary material solution and blank solvent methanol, injects liquid chromatograph,
Measure, collection of illustrative plates is recorded, as shown in Figure 4.
According to measurement result, auxiliary material with blank solvent in peak position without absworption peak, it is noiseless to assay.
Embodiment 5：Cefaclor equation of linear regression
Reference substance Cefaclor is configured to the standard liquid of the μ g/ml of 0.1mg/ml ~ 0.6 6 various concentrations respectively, according to reality
The chromatographic condition of example 1 is applied, each precision measures 10 μ L injection liquid chromatographs, records chromatogram, peak area is determined, with peak area value
（S）To concentration（C）Linear regression is carried out, tries to achieve the equation of linear regression of Cefaclor：y = 2,339,110.2857 x -
28,344.9333 R 2=1.0000 is linear good.And concentration C is mapped with peak area value S, a rectilinear is obtained, sees Fig. 5.
Embodiment 6：Bromhexine hydrochloride equation of linear regression
The standard that reference substance bromhexine hydrochloride is configured to 0.004mg/ml ~ 0.024mg/ml 10 various concentrations respectively is molten
Liquid, according to the chromatographic condition of embodiment 1, each precision measures 10 μ L injection liquid chromatographs, records chromatogram, determines peak area,
With peak area value（S）To concentration（C）Linear regression is carried out, tries to achieve the equation of linear regression of bromhexine hydrochloride：y = 11,440,
278.5714 x -35,074.7333 R2=0.9991 are linear good.And concentration C is mapped with peak area value S, obtain always
Line chart, see Fig. 6.
Embodiment 7：Sample introduction precision test
Reference substance solution preparation method and chromatographic condition take reference substance solution, continuous sample introduction 5 times, record chromatogram with embodiment 1
Figure, measurement result are shown in Table 1.
The sample introduction Precision test result of table 1
Conclusion：From table 1, result of the test Cefaclor RSD% is 0.1%（n=5）, bromhexine hydrochloride RSD% be 0.4%（n=
5）, show that sample introduction precision is preferable.
Embodiment 8：Recovery test
Cefaclor, bromhexine hydrochloride is taken to be made into contrast solution, chromatographic condition and detection side of each sample according to embodiment 1 respectively
Method determines, and calculates the rate of recovery, and measurement result is shown in Table 2, table 3.
The Cefaclor recovery test result of table 2
The bromhexine hydrochloride recovery test result of table 3
Conclusion：By table 2, table 3 is visible, and Cefaclor average recovery rate is 99.44%, RSD 2.10%, and bromhexine hydrochloride averagely returns
Yield is 96.97%, RSD 2.59%, shows that the rate of recovery is preferable.
Embodiment 9：Replica test
According to the chromatographic condition of embodiment 1,6 parts of sample for taking lot number to be 20160421, accurately weighed, measurement result is filtered respectively
It is shown in Table 4.
4 repeated measurement result of table（n=6）
Conclusion：From table 4, result of the test Cefaclor RSD is 1.58%, and bromhexine hydrochloride RSD is 2.03%, shows to repeat
Property is preferable.
Embodiment 10：Chromatographic condition durability change in flow
According to the experimental method of embodiment 1, flow velocity is changed into：0.9ml/min, 1.1ml/min, investigate Cefaclor and hydrochloric acid bromine
Peak separating degree between oneself is new, the results are shown in Table 5.
The change in flow test result table of table 5
Conclusion：Determined under this chromatographic condition, it is seen that change flow velocity in the range of 0.9ml/min ~ 1.1ml/min conditions permits
Separating degree detection is had not significant impact.
Embodiment 11：Chromatographic condition durability sample size changes
According to the experimental method of embodiment 1, sample size is changed into：8 μ l, 12 μ l are investigated between Cefaclor and bromhexine hydrochloride
Peak separating degree, the results are shown in Table 6.
The sample size of table 6 changes test result table
Conclusion：Determined under this chromatographic condition, it is seen that by flow velocity, change detects to separating degree in the range of the μ l conditions permits of 8 μ l ~ 12
Have not significant impact.
Embodiment 12：Chromatographic condition durability column temperature changes
According to the experimental method of embodiment 1, sample size is changed into：35 DEG C, 45 DEG C are investigated between Cefaclor and bromhexine hydrochloride
Peak separating degree, the results are shown in Table 7.
The sample size of table 7 changes test result table
Conclusion：Determined under this chromatographic condition, it is seen that flow velocity is changed in the range of 35 DEG C ~ 45 DEG C conditions permits separating degree is examined
Survey has not significant impact.
Claims (4)
- A kind of 1. method for determining plurality of active ingredients in the own new tablets of clo, it is characterised in that comprise the following steps：The preparation of reference substance solution：Cefaclor reference substance, bromhexine hydrochloride reference substance plus methanol dissolving are weighed, every 1mL is made Mixed reference substance solution containing μ g of Cefaclor 500, the μ g of bromhexine hydrochloride 20；The preparation of need testing solution：Take the own new tablets of clo appropriate, add methanol to dissolve, filter and produce；Chromatographic condition is as follows：Chromatographic column：Octadecyl silane chromatographic column；Mobile phase：0.005mol/L TBAHs, PH are adjusted to 3.2 ± 0.1 aqueous solution-methanol=45：55；Flow velocity：0.9mL/min ~1.1mL/min；Detection wavelength：240 ~ 245nm column temperatures：35℃ ~45℃；Sample size：8μL ~12μL；Theoretical cam curve：Calculated with Cefaclor peak and be more than or equal to 2000；Detection method：Precision draws reference substance solution and need testing solution, injects high performance liquid chromatograph, measure, records collection of illustrative plates, The collection of illustrative plates of reference substance and test sample is produced, compares Cefaclor, bromhexine hydrochloride equation of linear regression, to head in need testing solution Spore clo, bromhexine hydrochloride carry out qualitative and quantitative, and then calculate to obtain Cefaclor in the own new tablets of clo, bromhexine hydrochloride Content.
- 2. the method for plurality of active ingredients in the measure own new tablets of clo according to claim 1, it is characterised in that：It is described Mobile phase is 0.005mol/L TBAHs, and PH is adjusted to 3.2 aqueous solution-methanol=45：55, column temperature is 40 DEG C, inspection Survey wavelength is 243nm.
- 3. the method for plurality of active ingredients in the measure own new tablets of clo according to claim 1, it is characterised in that：It is described Mobile phase is 0.005mol/L TBAHs, and PH is adjusted to 3.1 aqueous solution-methanol=45：55, column temperature is 35 DEG C, inspection Survey wavelength is 240nm.
- 4. the method for plurality of active ingredients in the measure own new tablets of clo according to claim 1, it is characterised in that：It is described Mobile phase is 0.005mol/L TBAHs, and PH is adjusted to 3.3 aqueous solution-methanol=45：55, column temperature is 45 DEG C, inspection Survey wavelength is 245nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710885726.1A CN107807191A (en) | 2017-09-27 | 2017-09-27 | A kind of method for determining plurality of active ingredients in the own new tablets of clo |
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| CN201710885726.1A CN107807191A (en) | 2017-09-27 | 2017-09-27 | A kind of method for determining plurality of active ingredients in the own new tablets of clo |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115876900A (en) * | 2021-09-28 | 2023-03-31 | 江苏正大清江制药有限公司 | Method for measuring dissolution amount of bromhexine hydrochloride in clohexine dry suspension |
-
2017
- 2017-09-27 CN CN201710885726.1A patent/CN107807191A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 农业部农药检定所: "《假劣农药鉴定技术手册》", 30 September 2006, 中国农业出版社 * |
| 朱友林 等: "高效液相色谱法同时测定克洛己新干混悬剂中头孢克洛和盐酸溴己新的含量", 《中国医药导报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115876900A (en) * | 2021-09-28 | 2023-03-31 | 江苏正大清江制药有限公司 | Method for measuring dissolution amount of bromhexine hydrochloride in clohexine dry suspension |
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Application publication date: 20180316 |