CN102636582B - 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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- CN102636582B CN102636582B CN2012100702113A CN201210070211A CN102636582B CN 102636582 B CN102636582 B CN 102636582B CN 2012100702113 A CN2012100702113 A CN 2012100702113A CN 201210070211 A CN201210070211 A CN 201210070211A CN 102636582 B CN102636582 B CN 102636582B
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- antipyrine
- nitrogen
- diminazene
- amidine
- amidines
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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 three nitrogen amidines and antipyrine content in the quantitative measurement preparation, specifically with the method for three nitrogen amidines and antipyrine content in a kind of mensuration three nitrogen amidine granules.
Background technology
Three nitrogen amidines belong to the two amidine classes of fragrance, are the anti-Blood protozoan medicines of wide spectrum that tradition is used, and domestic animal pyriform worm, trypanosome and incorporeity are all had therapeutic action, but preventive effect are poor.The pest-resistant effect of the two amidine classes of fragrance is synthetic relevant with the aerobic glycolysis of disturbing polypide and DNA, and this class 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 class medicine.Three nitrogen amidine granules with therapeutic action, the inside has been added a certain amount of antipyrine and has been widely used by foreign market as the active substance of analgesic throe, but the liquid phase process that detects three nitrogen amidines and antipyrine in the three nitrogen amidine particles of document record at present 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 problem to be solved in the present invention, for having added the antipyrine active substance in three nitrogen amidine particles, there is no its detection method in Chinese Pharmacopoeia and bibliographical information, in the case, the assay method of measuring three nitrogen amidines and antipyrine content in a kind of mensuration three nitrogen amidine particles is provided, it is the HPLC method that the method belongs to high performance liquid chromatography, has the characteristics such as easy and simple to handle, accurate, good reproducibility, specificity are strong, is applicable to measure in three nitrogen amidine particles the mensuration of three nitrogen amidines and antipyrine content.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
The method of the content of three nitrogen amidines and antipyrine in a kind of mensuration three nitrogen amidine particles, it belongs to the HPLC method, and the chromatographic condition of the method is:
(1) be filling agent Diamonsil C with octadecylsilane chemically bonded silica
18Post (250mm * 4.6mm, 5 μ m);
(2) mobile phase volume is than being phosphate buffered solution: methyl alcohol=27:10;
(3) the detection wavelength of UV-detector is 250nm.
As a kind of restriction of the present invention, described phosphate buffer is potassium dihydrogen phosphate or sodium dihydrogen phosphate.
As the further restriction of above-mentioned restriction, described phosphate buffer is potassium dihydrogen phosphate.
As the restriction again of above-mentioned restriction, described potassium dihydrogen phosphate is 1.15% potassium dihydrogen phosphate aqueous solution.
As the last restriction of above-mentioned restriction, described potassium dihydrogen phosphate aqueous solution is with 85% phosphorus acid for adjusting pH value to 3.0.
As another kind of restriction the of the present invention, the chromatographic condition of described this HPLC method is: the flow velocity of mobile phase used is 0.5mL/min, and sampling volume is 20 μ L, and column temperature is 30 ℃.
By the said method of setting up, be used for measuring the content of three nitrogen amidines and antipyrine in three nitrogen amidine particles, can reach and analyze purpose accurately.
Owing to having adopted above-mentioned technical scheme, compared with prior art, obtained technical progress is in the present invention: the method for three nitrogen amidines and antipyrine content in employing HPLC method detection three nitrogen amidine particles, and simple to operate, improved the sensitivity and the accuracy that detect.
The present invention is suitable for the content of three nitrogen amidines and antipyrine in three nitrogen amidine particles is carried out HPLC method mensuration.
Description of drawings
Fig. 1 is the HPLC figure of embodiment of the present invention solvent interference test;
Fig. 2 is the HPLC figure of the blank auxiliary material interference test of the embodiment of the present invention;
Fig. 3 is the embodiment of the present invention three nitrogen amidine reference substance HPLC figure;
Fig. 4 is embodiment of the present invention antipyrine reference substance HPLC figure;
Fig. 5 is the embodiment of the present invention three nitrogen amidines and antipyrine standard items HPLC figure;
Fig. 6 is the embodiment of the present invention three nitrogen amidines and antipyrine sample HPLC figure;
Fig. 7 is the HPLC figure of embodiment of the present invention reference substance sample size 5 μ L linear determinations;
Fig. 8 is the HPLC figure of embodiment of the present invention reference substance sample size 10 μ L linear determinations;
Fig. 9 is the HPLC figure of embodiment of the present invention reference substance sample size 15 μ L linear determinations;
Figure 10 is the HPLC figure of embodiment of the present invention reference substance sample size 20 μ L linear determinations;
Figure 11 is the HPLC figure of embodiment of the present invention reference substance sample size 25 μ L linear determinations.
The present invention is described in further detail below in conjunction with Figure of description and specific embodiment.
Embodiment
Following examples are used for supplementary notes the present invention, and are not restriction of the present invention.
The method of three nitrogen amidines and antipyrine content in a kind of mensuration of embodiment three nitrogen amidine granules
The method belongs to the HPLC method, and its chromatographic condition is:
(1) be filling agent Diamonsil C with octadecylsilane chemically bonded silica
18Post (250mm * 4.6mm, 5 μ m);
(2) mobile phase volume is phosphate buffered solution: 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 mobile phase used 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: Shimadzu 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), three nitrogen amidine particles (sample, Hebei Kexing Drug Industry Co., Ltd. produces), three nitrogen amidine reference substance (lot numbers: 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 three nitrogen amidines, the characteristic that the antipyrine UV Absorption has, measured the absorption collection of illustrative plates of its aqueous solution under ultraviolet light, and three nitrogen amidines and antipyrine are that 250nm all has good absorption at wavelength, and intersect, and determines that therefore 250nm detects wavelength as it.
2.2, the preparation of solution
Solvent is mobile phase.
Mix the preparation of reference substance solution: precision takes three nitrogen amidine reference substance 40.0mg and antipyrine reference substance 55.0mg is placed in the brown volumetric flask of 100ml, with mobile phase, dissolves and is diluted to scale, shakes up and namely obtains reference substance solution M.
Three nitrogen amidine reference substance solution preparations: precision takes three nitrogen amidine reference substance 40.0mg and is placed in the brown volumetric flask of 100mL, with mobile phase, dissolves and is diluted to scale, shakes up and namely obtains solution A.
The preparation of antipyrine reference substance solution: precision takes antipyrine reference substance 55.0mg and is placed in the brown volumetric flask of 100mL, with mobile phase, dissolves and is diluted to scale, shakes up and namely obtains solution B.
The preparation of sample solution: precision takes sample appropriate (approximately be equivalent to three nitrogen amidine 40.0mg, antipyrine is about 55.0mg), is placed in the brown volumetric flask of 100mL, with mobile phase, dissolves and is diluted to scale, shakes up and namely obtains sample solution D.
2.3, the interference test of solvent, blank auxiliary material
, for getting rid of in chromatogram the appearance that has solvent and blank auxiliary material to disturb three nitrogen amidines and antipyrine peak, independent solvent and blank auxiliary material are carried out the specificity test, to increase the accuracy that detects.
The impact of solvent: get the mobile phase filtration and namely obtain sample 1.
The impact of blank auxiliary material: in the ratio of pharmaceutical formulation regulation, except three nitrogen amidines and antipyrine, add other auxiliary materials to make sample, precision takes this sample 0.1g and is placed in the brown volumetric flask of 100mL and dissolves with mobile phase and be diluted to scale, shake up, filter and namely obtain sample 2.
According to above-mentioned chromatographic condition sample introduction, difference sample thief 1 and sample 2 each 20 μ L, sample introduction, record chromatogram, as depicted in figs. 1 and 2.
Result shows: testing result does not have Interference Peaks to occur close to baseline as seen from Figure 1, shows the mensuration not impact of solvent on three nitrogen amidines and antipyrine.
Do not have as seen from Figure 2 Interference Peaks to occur, show the mensuration not impact of blank auxiliary material on three nitrogen amidines and antipyrine.
According to above-mentioned chromatographic condition sample introduction, get respectively each the 20 μ L of solution A, B, M and solution D under 2.2, sample introduction, record chromatogram, as Fig. 3-shown in Figure 6.Result shows: by Fig. 5 and Fig. 6, can find out in sample drawing that in antipyrine and three nitrogen amidine main peak retention times and standard items figure, antipyrine is consistent with three nitrogen amidine main peak retention times.
2.4, the mensuration of sample size
With the reference substance solution M for preparing, get 20 μ L sample introductions, get three batch samples, prepare sample solution according to above-mentioned 2.2 methods, every batch sample do 2 parallel, respectively get 20 μ L sample introductions, and record each main peak area and calculate the content of three nitrogen amidines and antipyrine by external standard method, result is as shown in table 1, and according to the test determination result, the content of determining three nitrogen amidines and antipyrine is the 90.0%-110.0% of labelled amount.
2.5, the specificity of method
, can degrade in the process of operation in more responsive to airborne oxygen, light and heat due to the characteristics of three nitrogen amidines itself, avoid the interference of catabolite to chromatographic peak, now carry out the separation under destructive test, verify detection method.
Separation under destructive test: get 5 groups of the required test samples of this assay, every group 3 parallel, be placed in 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% hydrogen peroxide), thermal environment (60 ℃) and luminous environment (4000L μ X), destroy 3h, get each the 20 μ L of sample after destruction, sample introduction.
Experimental result shows, 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 according to above-mentioned chromatographic condition injection liquid chromatography, and record chromatogram: the HPLC figure of the reference substance solution of above-mentioned different sample sizes is respectively as shown in Fig. 7-11.Linear relationship between calculating concentration and peak area, obtain regression curve and regression equation, and with peak area (A), sample size (C) is carried out linear regression, obtains three nitrogen amidine normal linearity equations to be: A=1909043C+449493; R=0.9991, result shows three nitrogen amidines in 2.3 μ g-11.6 μ g scopes, linear relationship is good; Obtaining antipyrine normal linearity equation with method is:
A=4670297C-250541, r=0.9999, result shows that antipyrine is good in 3.0 μ g-14.9 μ g scope internal linear relations, reference substance range of linearity measurement result is as shown in table 2.
2.7, the determining of detection line and quantitative limit
With the reference substance solution stepwise dilution, sample introduction, record peak height, and during concentration when peak height while being 10 times high of baseline noise, three nitrogen amidine quantitative limit concentration are 0.10 μ g/mL; Antipyrine quantitative limit concentration is 0.15 μ g/mL.The detectability concentration of three nitrogen amidines 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, according to above-mentioned chromatographic condition continuous sample introduction 5 times, and calculate the precision of the method.Test result is as shown in table 3, records the relative standard deviation RSD ﹤ 2% of three nitrogen amidines 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 respectively sample introduction after 0h, 2h, 4h, 6h and 8h 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 three nitrogen amidines and antipyrine peak area, illustrate that need testing solution is stable in 8h.
2.10, replica test
Precision takes 5 parts of same lot number three nitrogen amidine particulate samples, measures its content, and three nitrogen amidines and antipyrine average content are 96.0%, 102.1% as a result, and 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 measures totally 9 parts of blank auxiliary material 1ml, is placed in respectively the brown volumetric flask of 100mL, is divided into 3 groups, every group 3 parts, every group adds respectively three nitrogen amidine reference substance 32mg, 40mg, 48mg, (approximately be equivalent to 80%, 100% of three nitrogen amidine labelled amounts, 120%) and antipyrine reference substance 44mg, 55mg, 66mg (approximately is equivalent to 80% of antipyrine labelled amount, 100%, 120%), with mobile phase, dissolve and be diluted to scale, shake up, obtain.
Reference substance solution: precision takes the brown volumetric flask that three nitrogen amidine reference substance 40mg and antipyrine reference substance 55mg be placed in 100mL and dissolves with mobile phase and be diluted to scale, shakes up, and obtains.
According to said method, measure the content of three nitrogen amidines and antipyrine, be calculated as follows the recovery, result is as shown in table 6, shows that the three average average recoveries of nitrogen amidine are 99.5%(n=9), RSD is 0.49%; The average average recovery of antipyrine is that 100.0%, RSD is 0.49%, illustrates that its recovery is qualified.
The recovery of three nitrogen amidines (%)=
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 respectively three nitrogen amidine reference substance 32mg, 40mg, 48mg(approximately be equivalent to three nitrogen amidine labelled amounts 80%, 100%, 120%) and antipyrine reference substance 44mg, 55mg, 66mg (approximately be equivalent to antipyrine labelled amount 80%, 100%, 120%) dissolves with mobile phase and is diluted to scale, shake up, obtain.
Reference substance solution: precision takes the brown volumetric flask that three nitrogen amidine reference substance 40mg and antipyrine reference substance 55mg be placed in 100mL and dissolves with mobile phase and be diluted to scale, shakes up, and obtains reference substance solution.
According to said method, measure the content of three nitrogen amidines and antipyrine, calculate recovery rate, result is as shown in table 7, shows that three nitrogen amidine average recovery rates are 100.1%(n=9), the mean value of RSD is 0.60%; The antipyrine average recovery rate is that the mean value of 100.6%, RSD is 0.49%, and experimental result shows that its recovery is qualified.
Two, actual measurement
According to following detection method, three nitrogen amidines and antipyrine in 4 batches of three nitrogen amidine 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 mix, and with 85% phosphorus acid for adjusting pH value to 3.0, are mobile 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 and is not less than 1500 by three nitrogen amidine peaks, 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 in three nitrogen amidine reference substance 40.0mg and antipyrine reference substance 55.0mg to 100mL volumetric flask, with mobile phase, dissolves and is diluted to scale, shakes up and namely obtains reference substance solution M1.
The preparation of sample solution: precision takes sample appropriate (approximately being equivalent to three nitrogen amidine 40.0mg and antipyrine 55mg) to the 100mL volumetric flask, with mobile phase, dissolves and is diluted to scale, shakes up and namely obtains 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, with the content of external standard method by calculated by peak area three nitrogen amidines and antipyrine.Three nitrogen amidine main peak retention times are 7min, and the retention time of antipyrine main peak is 26min.Assay the results are shown in following table:
Claims (3)
1. method of measuring three nitrogen amidines and antipyrine content in three nitrogen amidine particles, it is characterized in that: it belongs to the HPLC method, and the chromatographic condition of the method is:
(1) be filling agent 250mm * 4.6mm with octadecylsilane chemically bonded silica, the Diamonsil C of 5 μ m
18Post;
(2) mobile phase volume is than being phosphate buffered solution: methyl alcohol=27:10;
(3) the detection wavelength of UV-detector is 250nm;
Wherein, described phosphate buffer is potassium dihydrogen phosphate; Potassium dihydrogen phosphate aqueous solution is with 85% phosphorus acid for adjusting pH value to 3.0.
2. the method for three nitrogen amidines and antipyrine content in mensuration three nitrogen amidine particles according to claim 1, it is characterized in that: described potassium dihydrogen phosphate concentration is 1.15% potassium dihydrogen phosphate aqueous solution.
3. the method for three nitrogen amidines and antipyrine content in mensuration three nitrogen amidine particles according to claim 1 and 2, it is characterized in that the chromatographic condition of the method is: the flow velocity of mobile phase used is 0.5mL/min, and sampling volume is 20 μ L, and column temperature is 30 ℃.
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Families Citing this family (3)
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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 |
| 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 |
| CN112526020B (en) * | 2020-11-27 | 2022-12-27 | 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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| DE19826793A1 (en) * | 1998-06-16 | 1999-12-23 | Chambord Ltd | Stable diminazene diaceturate preparation having antiprotozoal activity, used e.g. for treating malaria or trypanosomiasis |
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|---|---|---|---|---|
| DE19853937A1 (en) * | 1998-11-24 | 2000-05-25 | Chambord Ltd | Composition useful for treating e.g. malaria, babesiosis and trypanosomiasis comprises diminazene diaceturate and procaine |
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|---|---|---|---|---|
| DE19826793A1 (en) * | 1998-06-16 | 1999-12-23 | Chambord Ltd | Stable diminazene diaceturate preparation having antiprotozoal activity, used e.g. for treating malaria or trypanosomiasis |
| CN101129328A (en) * | 2007-09-13 | 2008-02-27 | 天津药业集团新郑股份有限公司 | Compound aminophenazone barbital Injection and method of producing the same |
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