CN102636582A - Method for determining content of diminazene and antipyrine in diminazene particle - Google Patents
Method for determining content of diminazene and antipyrine in diminazene particle Download PDFInfo
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- CN102636582A CN102636582A CN2012100702113A CN201210070211A CN102636582A CN 102636582 A CN102636582 A CN 102636582A CN 2012100702113 A CN2012100702113 A CN 2012100702113A CN 201210070211 A CN201210070211 A CN 201210070211A CN 102636582 A CN102636582 A CN 102636582A
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Abstract
The invention discloses a method for determining content of diminazene and antipyrine in diminazene particles, and belongs to HPLC (high performance liquid chromatography). The chromatographic conditions of the method is as follows: (1) octadecyl silane-bonded silica gel is DiamonsilC18 column (250mm*4.6mm, 5 mum) of a filler; (2) the mobile phase volume ratio of phosphate buffered saline to carbinol is 27 to 10; and (3) the measurement wavelength of an ultraviolet detector is 250nm, the flow velocity of the mobile phase is 0.5mL/min, the introduced sample volume is 20 muL, and the column temperature is 30 DEG C. The detection method disclosed by the invention is simple in operation, and enhance the sensitivity and the accuracy of the detection. The method disclosed by the invention is suitable for determining the content of diminazene and antipyrine in diminazene particles.
Description
Technical field
The invention belongs to the analytical chemistry field, relate to the method for Diminazene Aceturate and antipyrine content in the quantitative measurement preparation, specifically with a kind of method of measuring Diminazene Aceturate and antipyrine content in the Diminazene Aceturate granule.
Background technology
Diminazene Aceturate belongs to the two amidine classes of fragrance, is the anti-blood protozoon of the wide spectrum medicine that tradition is used, and domestic animal pyriform worm, trypanosome and incorporeity are all had therapeutic action, but preventive effect is relatively poor.The pest-resistant effect of the two amidine classes of fragrance is synthetic relevant with DNA with the aerobic glycolysis of disturbing polypide, and this type medicine all can cause host's hypoglycemia.The aerobic glycolysis that pyriform worm and trypanosome are carried out will rely on host's glucose, and its inhibiting effect and nucleoprotein denaturation to trypanosome aerobic glycolysis is depended in the trypanocidia effect of this type medicine.Diminazene Aceturate granule with therapeutic action; It is widely-used by the foreign market as the active substance of analgesic throe that a certain amount of antipyrine has been added in the inside; But the liquid phase process that detects Diminazene Aceturate and antipyrine in the Diminazene Aceturate of the document record at present particle also seldom has report, and pharmacopeia is not put down in writing the detection method of this kind yet both at home and abroad.
Summary of the invention
The technical matters that the present invention will solve; Be to have added the antipyrine active substance, do not have its detection method in Chinese Pharmacopoeia and the bibliographical information, in the case in the Diminazene Aceturate particle; Provide and measured Diminazene Aceturate and antipyrine Determination on content method in a kind of mensuration Diminazene Aceturate particle; It is the HPLC method that this method belongs to high performance liquid chromatography, has characteristics such as easy and simple to handle, accurate, good reproducibility, specificity are strong, is applicable to and measures Diminazene Aceturate and antipyrine Determination on content in the Diminazene Aceturate particle.
For solving the problems of the technologies described above, the technical scheme that the present invention adopted is:
A kind of method of measuring the content of Diminazene Aceturate and antipyrine in the Diminazene Aceturate particle, it belongs to the HPLC method, and the chromatographic condition of this method is:
(1) use octadecylsilane chemically bonded silica to be filling agent Diamonsil C
18Post (250mm * 4.6mm, 5 μ m);
(2) mobile phase volume is than being PBS: methyl alcohol=27:10;
(3) the detection wavelength of UV-detector is 250nm.
As a kind of qualification of the present invention, described phosphate buffer is potassium dihydrogen phosphate or sodium dihydrogen phosphate.
As the further qualification of above-mentioned qualification, described phosphate buffer is a potassium dihydrogen phosphate.
As the qualification once more of above-mentioned qualification, described potassium dihydrogen phosphate is 1.15% potassium dihydrogen phosphate aqueous solution.
As the last qualification of above-mentioned qualification, said potassium dihydrogen phosphate aqueous solution is with 85% phosphorus acid for adjusting pH value to 3.0.
As another kind of qualification the of the present invention, the chromatographic condition of said this HPLC method is: the flow velocity of used moving phase is 0.5mL/min, and sampling volume is 20 μ L, and column temperature is 30 ℃.
Through the said method of setting up, be used for measuring the content of Diminazene Aceturate and antipyrine in the Diminazene Aceturate particle, can reach and analyze purpose accurately.
Owing to adopted above-mentioned technical scheme, the present invention compared with prior art, the technical progress that is obtained is: adopt the HPLC method to detect the method for Diminazene Aceturate and antipyrine content in the Diminazene Aceturate particle, simple to operate, improved the sensitivity and the accuracy of detection.
The present invention is suitable for the content of Diminazene Aceturate and antipyrine in the Diminazene Aceturate particle is carried out HPLC method mensuration.
Description of drawings
Fig. 1 is the HPLC figure of embodiment of the invention solvent interference test;
Fig. 2 is the HPLC figure of the blank auxiliary material interference test of the embodiment of the invention;
Fig. 3 is embodiment of the invention Diminazene Aceturate reference substance HPLC figure;
Fig. 4 is embodiment of the invention antipyrine reference substance HPLC figure;
Fig. 5 is embodiment of the invention Diminazene Aceturate and antipyrine standard items HPLC figure;
Fig. 6 is embodiment of the invention Diminazene Aceturate and antipyrine sample HPLC figure;
Fig. 7 is the HPLC figure of embodiment of the invention reference substance sample size 5 μ L linear determinations;
Fig. 8 is the HPLC figure of embodiment of the invention reference substance sample size 10 μ L linear determinations;
Fig. 9 is the HPLC figure of embodiment of the invention reference substance sample size 15 μ L linear determinations;
Figure 10 is the HPLC figure of embodiment of the invention reference substance sample size 20 μ L linear determinations;
Figure 11 is the HPLC figure of embodiment of the invention reference substance sample size 25 μ L linear determinations.
The present invention below will combine Figure of description and specific embodiment to do further explain.
Embodiment
Following examples are used to the present invention that remarks additionally, and are not qualification of the present invention.
Embodiment is a kind of to measure the method for Diminazene Aceturate and antipyrine content in the Diminazene Aceturate granule
This method belongs to the HPLC method, and its chromatographic condition is:
(1) use octadecylsilane chemically bonded silica to be filling agent Diamonsil C
18Post (250mm * 4.6mm, 5 μ m);
(2) mobile phase volume is PBS: methyl alcohol=27:10.Phosphate buffer is potassium dihydrogen phosphate (also can substitute with sodium dihydrogen phosphate), is specially 1.15% potassium dihydrogen phosphate aqueous solution, with 85% phosphorus acid for adjusting pH value to 3.0;
The flow velocity of used moving phase is 0.5mL/min, and sampling volume is 20 μ L, and column temperature is 30 ℃;
(3) the detection wavelength of UV-detector is 250nm.
One, the process of setting up of the inventive method:
1, instrument and reagent
Instrument: Tianjin, island LC-2010A high performance liquid chromatograph (LC-2010 model detecting device, LC-2010 model pump, LC-2010 column oven, LC-2010 automatic sampler), LCsolution chromatographic work station;
Reagent: methyl alcohol (chromatographically pure), potassium dihydrogen phosphate (top grade is pure), phosphoric acid (top grade is pure); Water (secondary deionized water); Diminazene Aceturate particle (sample, Hebei Kexing Drug Industry Co., Ltd. produces), Diminazene Aceturate reference substance (lot number: 091203; Nat'l Pharmaceutical & Biological Products Control Institute, content is 99.6%); Antipyrine reference substance (content is 99.8% for lot number: 100506-200301, Nat'l Pharmaceutical & Biological Products Control Institute).
2, the foundation of content assaying method
2.1, the selection of wavelength
According to Diminazene Aceturate, the characteristic that the antipyrine UV Absorption has has been measured the absorption collection of illustrative plates of its WS under ultraviolet light, and Diminazene Aceturate and antipyrine are that 250nm all has good absorption at wavelength, and intersects, and confirms that therefore 250nm detects wavelength as it.
2.2, the preparation of solution
Solvent is a moving phase.
Mix the preparation of reference substance solution: precision takes by weighing Diminazene Aceturate reference substance 40.0mg and antipyrine reference substance 55.0mg places the brown volumetric flask of 100ml, dissolves and is diluted to scale with moving phase, shakes up and promptly gets reference substance solution M.
Diminazene Aceturate reference substance solution preparation: precision takes by weighing Diminazene Aceturate reference substance 40.0mg and places the brown volumetric flask of 100mL, with the moving phase dissolving and be diluted to scale, shakes up and promptly gets solution A.
The preparation of antipyrine reference substance solution: precision takes by weighing antipyrine reference substance 55.0mg and places the brown volumetric flask of 100mL, with moving phase dissolving and be diluted to scale, shakes up and promptly gets solution B.
The preparation of sample solution: precision takes by weighing sample an amount of (be equivalent to Diminazene Aceturate 40.0mg approximately, antipyrine is about 55.0mg), places the brown volumetric flask of 100mL, with the moving phase dissolving and be diluted to scale, shakes up and promptly gets sample solution D.
2.3, the interference test of solvent, blank auxiliary material
For getting rid of the appearance that has solvent and blank auxiliary material to disturb Diminazene Aceturate and antipyrine peak in the chromatogram, independent solvent and blank auxiliary material are carried out the specificity test, to increase the accuracy that detects.
The influence of solvent: get the moving phase filtration and promptly get sample 1.
The influence of blank auxiliary material: in the ratio of pharmaceutical formulation regulation; Except that Diminazene Aceturate and antipyrine, add other auxiliary materials and process sample, precision takes by weighing this sample 0.1g and places the brown volumetric flask of 100mL with moving phase dissolving and be diluted to scale; Shake up, filter and promptly get sample 2.
According to above-mentioned chromatographic condition sample introduction, difference sample thief 1 and sample 2 each 20 μ L, sample introduction, the record chromatogram, as depicted in figs. 1 and 2.
The result shows: can find out that by Fig. 1 testing result approaches baseline and do not have Interference Peaks to occur, show the mensuration not influence of solvent to Diminazene Aceturate and antipyrine.
Can find out do not have Interference Peaks to occur by Fig. 2, show of the mensuration not influence of blank auxiliary material Diminazene Aceturate and antipyrine.
According to above-mentioned chromatographic condition sample introduction, get each the 20 μ L of solution A, B, M and solution D under 2.2 respectively, sample introduction, the record chromatogram is like Fig. 3-shown in Figure 6.The result shows: can find out in the sample drawing that by Fig. 5 and Fig. 6 antipyrine is consistent with Diminazene Aceturate main peak retention time in the antipyrine and Diminazene Aceturate main peak retention time and standard items figure.
2.4, the mensuration of sample size
With the reference substance solution M for preparing, get 20 μ L sample introductions, get three lot sample article; Prepare sample solution according to above-mentioned 2.2 methods, every lot sample article do 2 parallel, respectively get 20 μ L sample introductions; And write down each main peak area and calculate the content of Diminazene Aceturate and antipyrine by external standard method; The result is as shown in table 1, and according to the test determination result, the content of confirming Diminazene Aceturate and antipyrine is the 90.0%-110.0% of labelled amount.
2.5, the specificity of method
Because the characteristic of Diminazene Aceturate itself can be degraded in the process of operation in relatively more responsive to airborne oxygen, light and heat, avoids the interference of catabolite to chromatographic peak, carries out the separation under the destructive test at present, the checking detection method.
Separation under the destructive test: get 5 groups of the required test samples of this assay; Every group 3 parallel; Place respectively under the condition of sour environment (hydrochloric acid solution of 0.1mol/L), alkaline environment (sodium hydroxide solution of 0.1mol/L), well-oxygenated environment (5% oxydol), thermal environment (60 ℃) and luminous environment (4000L μ X); Destroy 3h, get each the 20 μ L of sample after the destruction, sample introduction.
Experimental result shows that this preparation all has catabolite to generate under above-mentioned destructive condition, but catabolite and main peak all can reach separating effect preferably, and also separating effect preferably can be arranged between the catabolite peak.
2.6, the investigation of linear relationship and scope
Get reference substance solution M 5 μ L, 10 μ L, 15 μ L, 20 μ L and 25 μ L and inject liquid chromatograph according to above-mentioned chromatographic condition, and the record chromatogram: the HPLC figure of the reference substance solution of above-mentioned different sample sizes is respectively shown in Fig. 7-11.Linear relationship between calculating concentration and the peak area gets regression curve and regression equation, and with peak area (A) sample size (C) is carried out linear regression, gets Diminazene Aceturate normal linearity equation and is: A=1909043C+449493; R=0.9991, result show Diminazene Aceturate in 2.3 μ g-11.6 μ g scopes, and linear relationship is good; Getting antipyrine normal linearity equation with method is:
A=4670297C-250541, r=0.9999, the result shows that antipyrine is good in 3.0 μ g-14.9 μ g scope internal linear relation, it is as shown in table 2 that the reference substance range of linearity is measured the result.
2.7, the confirming of detection line and quantitative limit
With the reference substance solution stepwise dilution, sample introduction, the record peak height, Diminazene Aceturate quantitative limit concentration is 0.10 μ g/mL when the concentration of peak height when being 10 times high of baseline noise; Antipyrine quantitative limit concentration is 0.15 μ g/mL.The detectability concentration of Diminazene Aceturate is 0.03 μ g/mL when peak height is the concentration of baseline noise 2-3 when doubly high; The detection line concentration of antipyrine is 0.05 μ g/mL.
2.8, the investigation of precision test
Get each 20 μ L of 5 parts of reference substance solution M,, and calculate the precision of this method according to above-mentioned chromatographic condition continuous sample introduction 5 times.Test result is as shown in table 3, records the relative standard deviation RSD ﹤ 2% of Diminazene Aceturate and antipyrine, shows that the precision of this method is good.
2.9, stability test
Getting reference substance solution M and sample solution D places behind 0h, 2h, 4h, 6h and the 8h sample introduction respectively and measures; Each time period difference continuous sample introduction 3 times; Experimental result is as shown in table 4; And calculate the relative standard deviation RSD ﹤ 2% of Diminazene Aceturate and antipyrine peak area, explain that need testing solution is stable in 8h.
2.10, replica test
Precision takes by weighing 5 parts of same lot number Diminazene Aceturate particulate samples, measures its content, and Diminazene Aceturate and antipyrine average content are 96.0%, 102.1% as a result, and the result is as shown in table 5, relative standard deviation RSD＜2%.The repeatability of illustration method is good.
2.11, add the investigation of the recovery of blank auxiliary material
Need testing solution: precision is measured totally 9 parts of blank auxiliary material 1ml, places the brown volumetric flask of 100mL respectively, is divided into 3 groups, and 3 parts every group, every group adds Diminazene Aceturate reference substance 32mg respectively; 40mg, 48mg (is equivalent to 80%, 100% of Diminazene Aceturate labelled amount approximately; 120%) and antipyrine reference substance 44mg, 55mg, 66mg (is equivalent to 80%, 100% of antipyrine labelled amount approximately; 120%), with moving phase dissolving and be diluted to scale, shakes up, promptly get.
Reference substance solution: precision takes by weighing brown volumetric flask that Diminazene Aceturate reference substance 40mg and antipyrine reference substance 55mg place 100mL with the moving phase dissolving and be diluted to scale, shakes up, and promptly gets.
According to said method, measure the content of Diminazene Aceturate and antipyrine, be calculated as follows the recovery, the result is as shown in table 6, shows that the average average recovery of Diminazene Aceturate is 99.5% (n=9), and RSD is 0.49%; The average average recovery of antipyrine is 100.0%, and RSD is 0.49%, explains that its recovery is qualified.
The recovery of Diminazene Aceturate (%)=
The recovery of antipyrine (%)=
2.12, do not add the investigation of the recovery of blank auxiliary material
Need testing solution: test sample is divided into 3 groups, and 3 parts every group, every group adds Diminazene Aceturate reference substance 32mg, 40mg respectively; 48mg (be equivalent to approximately Diminazene Aceturate labelled amount 80%, 100%, 120%) and antipyrine reference substance 44mg; 55mg, 66mg (is equivalent to 80%, 100% of antipyrine labelled amount approximately; 120%) with moving phase dissolving and be diluted to scale, shake up, promptly get.
Reference substance solution: precision takes by weighing brown volumetric flask that Diminazene Aceturate reference substance 40mg and antipyrine reference substance 55mg place 100mL with the moving phase dissolving and be diluted to scale, shakes up, and promptly gets reference substance solution.
According to said method, measure the content of Diminazene Aceturate and antipyrine, calculate recovery rate, the result is as shown in table 7, shows that the Diminazene Aceturate average recovery rate is 100.1% (n=9), and the mean value of RSD is 0.60%; The antipyrine average recovery rate is 100.6%, and the mean value of RSD is 0.49%, and experimental result shows that its recovery is qualified.
Two, actual measurement
According to following detection method Diminazene Aceturate and antipyrine in 4 batches of Diminazene Aceturate particles are carried out assay.Utilize Diamonsil C
18Post (250mm * 4.6mm, 5 μ m); 1.15% potassium dihydrogen phosphate 675mL and 250mL methyl alcohol mixing use 85% phosphorus acid for adjusting pH value to 3.0 to be moving phase; The detection wavelength is 250nm; Flow velocity is 0.5ml/min, 30 ℃ of column temperatures, and sample size 20 μ L, theoretical cam curve is calculated by the Diminazene Aceturate peak and is not less than 1500, and the degree of separation of main peak and impurity peaks meets the requirements, and tailing factor is not more than 1.5.
The preparation of reference substance solution: precision takes by weighing in Diminazene Aceturate reference substance 40.0mg and antipyrine reference substance 55.0mg to the 100mL volumetric flask, with moving phase dissolving and be diluted to scale, shakes up and promptly gets reference substance solution M1.
The preparation of sample solution: precision takes by weighing sample an amount of (being equivalent to Diminazene Aceturate 40.0mg and antipyrine 55mg approximately) to the 100mL volumetric flask, dissolves and is diluted to scale with moving phase, shakes up and promptly gets sample solution D1.
Under chromatographic condition of the present invention, get each 20 μ L of above-mentioned sample solution and reference substance solution, sample introduction, record chromatogram main peak area is with the content of external standard method by calculated by peak area Diminazene Aceturate and antipyrine.Diminazene Aceturate main peak retention time is 7min, and the retention time of antipyrine main peak is 26min.Assay is the result see the following form:
Claims (6)
1. method of measuring Diminazene Aceturate and antipyrine content in the Diminazene Aceturate particle, it is characterized in that: it belongs to the HPLC method, and the chromatographic condition of this method is:
(1) use octadecylsilane chemically bonded silica to be filling agent Diamonsil C
18Post (250mm * 4.6mm, 5 μ m);
(2) mobile phase volume is PBS: methyl alcohol=27:10;
(3) the detection wavelength of UV-detector is 250nm.
2. the method for Diminazene Aceturate and antipyrine content in the mensuration Diminazene Aceturate particle according to claim 1 is characterized in that: described phosphate buffer is a kind of in potassium dihydrogen phosphate or the sodium dihydrogen phosphate.
3. the method for Diminazene Aceturate and antipyrine content in the mensuration Diminazene Aceturate particle according to claim 2, it is characterized in that: described phosphate buffer is a potassium dihydrogen phosphate.
4. the method for Diminazene Aceturate and antipyrine content in the mensuration Diminazene Aceturate particle according to claim 3 is characterized in that: described potassium dihydrogen phosphate concentration is 1.15% potassium dihydrogen phosphate aqueous solution.
5. the method for Diminazene Aceturate and antipyrine content in the mensuration Diminazene Aceturate particle according to claim 4, it is characterized in that: said potassium dihydrogen phosphate aqueous solution is with 85% phosphorus acid for adjusting pH value to 3.0.
6. according to the method for Diminazene Aceturate and antipyrine content in each described mensuration Diminazene Aceturate particle among the claim 1-5; The chromatographic condition that it is characterized in that this method is: the flow velocity of used moving phase is 0.5mL/min; Sampling volume is 20 μ L, and column temperature is 30 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105168121A (en) * | 2015-08-28 | 2015-12-23 | 重庆布尔动物药业有限公司 | Diminazene compound for veterinary use and preparation method of diminazene compound |
| CN106872629A (en) * | 2016-11-07 | 2017-06-20 | 上海德诺产品检测有限公司 | A kind of method of three nitrogen amidine contents in measure dairy products |
| CN112526020A (en) * | 2020-11-27 | 2021-03-19 | 欧陆分析检测技术服务(青岛)有限公司 | Method for detecting residual triazamidine |
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| WO2000030611A2 (en) * | 1998-11-24 | 2000-06-02 | Chambord Ltd. | Pharmaceutical preparation |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105168121A (en) * | 2015-08-28 | 2015-12-23 | 重庆布尔动物药业有限公司 | Diminazene compound for veterinary use and preparation method of diminazene compound |
| CN106872629A (en) * | 2016-11-07 | 2017-06-20 | 上海德诺产品检测有限公司 | A kind of method of three nitrogen amidine contents in measure dairy products |
| CN106872629B (en) * | 2016-11-07 | 2019-03-26 | 上海德诺产品检测有限公司 | A kind of method of three nitrogen amidine contents in measurement dairy products |
| CN112526020A (en) * | 2020-11-27 | 2021-03-19 | 欧陆分析检测技术服务(青岛)有限公司 | Method for detecting residual triazamidine |
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Effective date of registration: 20210106 Address after: 570145 room 1506, Yusha international, 11-8 Yusha Road, Longhua District, Haikou City, Hainan Province Patentee after: Quanku (Hainan) Intellectual Property Operation Co.,Ltd. Address before: 050200 No.114 Changsheng street, high tech Industrial Development Zone, Luquan City, Shijiazhuang City, Hebei Province Patentee before: HEBEI KEXING PHARMACEUTICAL Co.,Ltd. |
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Effective date of registration: 20210125 Address after: 050200 No.114 Changsheng street, Luquan Development Zone, Shijiazhuang City, Hebei Province Patentee after: HEBEI KEXING PHARMACEUTICAL Co.,Ltd. Address before: 570145 room 1506, Yusha international, 11-8 Yusha Road, Longhua District, Haikou City, Hainan Province Patentee before: Quanku (Hainan) Intellectual Property Operation Co.,Ltd. |
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Granted publication date: 20131113 |