CN109100455A - The content assaying method of Parvaquone in a kind of Parvaquone injection for animals - Google Patents
The content assaying method of Parvaquone in a kind of Parvaquone injection for animals Download PDFInfo
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- CN109100455A CN109100455A CN201811252955.0A CN201811252955A CN109100455A CN 109100455 A CN109100455 A CN 109100455A CN 201811252955 A CN201811252955 A CN 201811252955A CN 109100455 A CN109100455 A CN 109100455A
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- parvaquone
- injection
- animals
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- methanol
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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Abstract
The invention discloses a kind of content assaying methods of Parvaquone in Parvaquone injection for animals, are related to analytical chemistry field.Present invention be characterized in that carrying out constituent analysis with high performance liquid chromatography to the Parvaquone injection for animals containing Parvaquone, the high performance liquid chromatography: it is filled into the chromatographic column of liquid chromatograph using octadecylsilane chemically bonded silica as stationary phase；Its pH value as mobile phase and is adjusted to 3.6 using methanol -0.05mol/L sodium acetate solution, the volume ratio of methanol and 0.05mol/L sodium acetate solution is 85:15；Detection wavelength is 252nm；The column temperature of chromatographic column is maintained at 30 DEG C.By external standard method with calculated by peak area to get the content of Parvaquone in Parvaquone injection for animals.The present invention can accurately measure the Parvaquone content in Parvaquone injection for animals.
Description
Technical field
The present invention relates to analytical chemistry field, the assay side of Parvaquone in especially a kind of Parvaquone injection for animals
Method.
Background technique
The chemical name of Parvaquone is -3 hydroxyls of 2- cyclohexyl -1,4-naphthoquinone, is a kind of babesiasis of novel anti-ox
Drug, ox babesia taylor disease are that the various pyriform worms that Taylor section Taylor belongs to parasitize bovine red blood cells, macrophage and lymphocyte
In, cause a kind of disease of ox anaemia and lymph enlargement.Northwest China, North China, some provinces and regions in northeast are popular in, are a kind of seasonalities
Epidemic disease, is in acute process more, and disease incidence, case fatality rate are high.Northern China is fallen ill mostly in 6~August, and July is peak period.Parvaquone
Injection is a kind of novel drug, but at present document to the detection method of the Parvaquone content in Parvaquone injection without report
Road.
Summary of the invention
Technical problem to be solved by the invention is to provide the assays for measuring Parvaquone in Parvaquone injection for animals
Method, the present invention can accurately measure the Parvaquone content in Parvaquone injection.
In order to solve the above technical problems, the technical solution used in the present invention is: a kind of pa in Parvaquone injection for animals
Cut down the content assaying method of quinone, which is characterized in that the Parvaquone injection high performance liquid chromatography for animals containing Parvaquone into
Row constituent analysis, the high performance liquid chromatography:
It is filled into the chromatographic column of liquid chromatograph using octadecylsilane chemically bonded silica as stationary phase；
Its pH value as mobile phase and is adjusted to 3.6 using methanol -0.05mol/L sodium acetate solution, methanol and
The volume ratio of 0.05mol/L sodium acetate solution is 85:15；
Detection wavelength is 252nm；
The column temperature of chromatographic column is maintained at 30 DEG C.
A further technical solution lies in number of theoretical plate is calculated by Parvaquone is not less than 2000.
Further technical solution also resides in, and takes Parvaquone injection 1ml for animals, adds methanol to dissolve and quantifies dilution and is made
The solution of the Parvaquone containing 0.15mg in every 1ml, as test solution.
Further technical solution also resides in, and the sampling volume of the test solution is 20 μ l.
Further technical solution also resides in, flow velocity 1.0ml/min.
The beneficial effects of adopting the technical scheme are that compared with prior art, the present invention acquired skill
Art progress is: the present invention measures the content of Parvaquone in Parvaquone injection using the method for efficient liquid phase, easy to operate, fastly
Fast, reproducible, stability is good, specificity is strong, detection sensitivity with higher and accuracy.And it is obtained in practice in production
Verifying, become determine product whether He Ge important technical file and foundation, use, have suitable for quality control standard
Conducive to large scale application.
85:15 methanol -0.05mol/L sodium acetate solution is adjusted to 3.6 with pH value by the present invention, improves appearance well
Time and peak shape, not only shorten appearance time, save solvent, while effectively improving Parvaquone in liquid chromatogram
Peak shape keeps the peak area of Parvaquone obtained in liquid chromatogram more accurate, is more advantageous to the accurate survey to Parvaquone content
It is fixed.
Present invention methanol dissolves reference substance and preparation, with good stability, therefore the method for the present invention is suitable for connecting
The assay for continuing multiple samples waits upon and surveys solution without matching while using, and solution to be measured still can be with originally after placing a period of time
Method is measured, and saves the labor intensity of experimenter.
Detailed description of the invention
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is concentration-peak area curve graph；
Fig. 2 is Parvaquone injection high-efficient liquid phase chromatogram；
Specific embodiment
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground description, it is clear that described embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, but the present invention can be with
Implemented using other than the one described here other way, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by the specific embodiments disclosed below.
The present embodiment belongs to high performance liquid chromatography, chromatographic condition are as follows:
It (1) is filler with octadecylsilane chemically bonded silica；(pH value is adjusted with methanol -0.05mol/L sodium acetate solution
It is mobile phase to 3.6) (85:15)；
(2) Detection wavelength 252nm；
(3) column temperature: 30 DEG C
(4) flow velocity: 1.0ml/min
(5) sampling volume: 20 μ l
(6) number of theoretical plate is calculated by Parvaquone is not less than 2000.
The preparation of solution
(1) preparation of reference substance solution: taking reference substance appropriate, add methanol to dissolve and quantify dilution be made in every 1ml containing about
The solution of 0.15mg；
(2) preparation of test solution: taking test sample 1ml, add methanol to dissolve and quantify dilution be made in every 1ml containing about
The solution of 0.15mg；
Measurement: precision measures reference substance solution and each 20 μ l of test solution, injects liquid chromatograph, records chromatogram；
By external standard method with calculated by peak area to get the content of Parvaquone in test solution.
The selection of wavelength
According to the UV Absorption characteristic of Parvaquone, the absorption map of its methanol solution under ultraviolet light is determined, pa is cut down
It is to have absorption maximum under 252nm wavelength that quinone, which wants wavelength, it is thus determined that 252nm is as its Detection wavelength.
The test of the interference of diluent and blank auxiliary
In order to determine the accuracy of measuring method, diluent and blank auxiliary should not influence the appearance of main peak Parvaquone, existing
By the specificity test to diluent and blank auxiliary, accuracy is determined to increase detection.
The interference of diluent is tested: methanol being taken to cross 0.45 μm of filter membrane, 20 μ l of sample introduction.
The interference of blank auxiliary is tested: according to ratio specified in pharmaceutical formulation, in addition to Parvaquone, other auxiliary materials are added
Sample is made, 1ml is taken to set in the volumetric flask of 100ml, with methanol dilution to scale, shakes up, then accurate measurement 10ml, sets 100ml
Volumetric flask in, with methanol dilution to scale, 20 μ l of sample introduction.
1 specificity test result of table
From the measurement result of table 1 it can be seen that diluent and blank auxiliary do not influence the measurement of main peak.
System suitability: taking reference substance solution, and precision measures 20 μ l and injects liquid chromatograph, replication 6 times, is subjected to
Peak area RSD value is not greater than 2%
The measurement result of 2 system suitability of table
From table 2 it can be seen that the system suitability of this standard is good
Stability of solution: it takes test solution and control solution by above-mentioned chromatographic process, records chromatogram.From sample and
Reference substance starts after matching, and measures in a few days, investigates the stability of solution.
| Time | Parvaquone sample peak area | Parvaquone reference substance peak area |
| 0h | 260.4934 | 263.558 |
| 2h | 261.2513 | 265.009 |
| 4h | 260.852 | 264.347 |
| 6h | 260.924 | 264.339 |
| 8h | 261.639 | 264.557 |
| 10h | 261.649 | 264.900 |
| 12h | 262.024 | 265.176 |
| 14h | 262.997 | 265.346 |
| 16h | 263.177 | 265.209 |
| 18h | 263.693 | 265.389 |
| 20h | 264.187 | 265.446 |
| 22h | 265.065 | 264.526 |
| 24h | 264.754 | 265.032 |
| RSD value | 0.59% | 0.21% |
3 Parvaquone injection stability of solution measurement result of table
From table 3 it can be seen that RSD value≤2.0% of the Parvaquone solution being formulated at 24 hours, illustrate to prepare and
At Parvaquone solution be stable at least within 24 hours
The investigation of linear relationship and range: taking Parvaquone reference substance 30mg, set in 100ml measuring bottle, add methanol dissolve and it is dilute
It releases to scale (0.30mg/ml).Accurate measurement above-mentioned solution 3ml, 4ml, 5ml, 6ml, 7ml are set in 10ml measuring bottle respectively, are made
0.09mg/ml (60%), 0.12mg/ml (80%), 0.15mg/ml (100%), 0.18mg/ml (120%), 0.21mg/ml
(140%) solution.As linear test solution, precision measures 20 μ l and injects liquid chromatograph.
4 Parvaquone linear determination result of table
From table 4, Fig. 1 be can be seen that within the scope of 0.0934mg/ml~0.2180mg/ml, and linear relationship is good.
Repetitive test: repeatability is by configuring 6 parts of test solutions, and method is surveyed under product content determination item in the same old way
Fixed, every 2 needle of sample sample introduction is averaged calculating content, and the RSD value of 6 results of acceptable standard is not greater than 2.0%.
5 Parvaquone injection repeatability measurement result of table
As can be seen from Table 5, repeatability is good.
Intermediate precision test: Parvaquone content assaying method is shone, by configuring 6 parts of test solutions, by two differences
Analysis personnel be measured in accordance with the law using different instruments.Every sample is averaged calculating content, acceptable standard 6 into 2 needles
RSD value≤2.0% of secondary result, RSD value≤2.0% with repeated data.
6 Parvaquone injection Intermediate precision measurement result of table
As can be seen from Table 6, Intermediate precision is good.
Accuracy test (rate of recovery): accuracy is cut down by measuring the pa of 80%, 100%, 120% 3 various concentration
Ratio between quinone solution result and theoretical value, it is expressed as a percentage, it is desirable that the rate of recovery is between 98.0%~102.0%, and 9
The relative standard deviation (RSD) of rate of recovery data should be not more than 2.0%.
7 Parvaquone of table injects liquid yield measurement result
As can be seen from Table 7, for the rate of recovery between 98.0%~102.0%, the relative standard of 9 rate of recovery data is inclined
Poor (RSD) should be not more than 2.0%, meet verification condition.
Durability: will be by changing different flow velocity, different column temperatures, different wave length, mobile phase ratio and different batches
When chromatographic column has small variation to assess determination condition parameter, the impregnable Bearing degree of measurement result, it is desirable that Ge Gebian
Under dynamic chromatographic condition parameter, the separating degree of mixed solution meets regulation, and the tailing factor of main peak is not greater than 2.0, each condition
Under content data relative standard deviation should be not more than 2.0%
8 Parvaquone injection durability measurement result of table
As can be seen from Table 8, chromatographic condition occurs still to measure content well when minor change.
Measurement result: the measuring method of the content according to verifying carries out assay, five batches of contents to the sample of production
Respectively 100.9%, 98.2%, 99.3%, 101.1%, 99.6%.
Claims (5)
1. the content assaying method of Parvaquone in a kind of Parvaquone injection for animals, which is characterized in that the beast containing Parvaquone
Constituent analysis is carried out with Parvaquone injection with high performance liquid chromatography, the high performance liquid chromatography:
It is filled into the chromatographic column of liquid chromatograph using octadecylsilane chemically bonded silica as stationary phase；
Its pH value as mobile phase and is adjusted to 3.6 using methanol -0.05mol/L sodium acetate solution, methanol and 0.05mol/L vinegar
The volume ratio of acid sodium solution is 85:15；
Detection wavelength is 252nm；
The column temperature of chromatographic column is maintained at 30 DEG C.
2. the content assaying method of Parvaquone, feature exist in a kind of Parvaquone injection for animals according to claim 1
In: number of theoretical plate is calculated by Parvaquone is not less than 2000.
3. the content assaying method of Parvaquone, feature exist in a kind of Parvaquone injection for animals according to claim 1
In: Parvaquone injection 1ml for animals is taken, adds methanol to dissolve and quantifies the solution that the Parvaquone containing 0.15mg in every 1ml is made in dilution,
As test solution.
4. the content assaying method of Parvaquone, feature exist in a kind of Parvaquone injection for animals according to claim 3
In: the sampling volume of the test solution is 20 μ l.
5. the content assaying method of Parvaquone, feature exist in a kind of Parvaquone injection for animals according to claim 1
In: flow velocity 1.0ml/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811252955.0A CN109100455A (en) | 2018-10-25 | 2018-10-25 | The content assaying method of Parvaquone in a kind of Parvaquone injection for animals |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811252955.0A CN109100455A (en) | 2018-10-25 | 2018-10-25 | The content assaying method of Parvaquone in a kind of Parvaquone injection for animals |
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| CN109100455A true CN109100455A (en) | 2018-12-28 |
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| CN201811252955.0A Pending CN109100455A (en) | 2018-10-25 | 2018-10-25 | The content assaying method of Parvaquone in a kind of Parvaquone injection for animals |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104535680A (en) * | 2014-12-25 | 2015-04-22 | 河北科星药业有限公司 | Method for determining buparvaquone content in buparvaquone injection |
-
2018
- 2018-10-25 CN CN201811252955.0A patent/CN109100455A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104535680A (en) * | 2014-12-25 | 2015-04-22 | 河北科星药业有限公司 | Method for determining buparvaquone content in buparvaquone injection |
Non-Patent Citations (1)
| Title |
|---|
| L.D.B.KINABO ET AL.: "Parvaquone and buparvaquone：HPLC analysis and comparative pharmacokinetics in cattle", 《ACTA TROPICA》 * |
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