CN103645261B - A kind of Ce Dings the liquid phase chromatography analytical method of oxolinic acid content - Google Patents
A kind of Ce Dings the liquid phase chromatography analytical method of oxolinic acid content Download PDFInfo
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Abstract
The invention discloses a kind of Ce and Ding the liquid phase chromatography analytical method of oxolinic acid content, belong to medication chemistry technical field of quality detection.The method comprises: be dissolved in by Dai Ce oxolinic acid sample in the mixed solvent of dimethyl formamide and methyl alcohol 2:3 ~ 5 by volume and obtain sample solution; Adopt the content of external standard method sample solution Zhong oxolinic acid, its chromatographic condition is: chromatographic column is C18 post, mobile phase: acetonitrile, the organic modifiers adding organic base and interpolation organic acid water are the mixed solution that 10 ~ 30:5 ~ 20:60 ~ 90 form by volume, flow velocity: 0.3 ~ 1.2mL/min, determined wavelength: 300 ~ 350nm, column temperature: 35 ~ 45 DEG C, sample size: 5 ~ 20 μ L.Adopt method Ke Shi oxolinic acid provided by the invention to be effectively separated with impurity A, B, C, the content of Accurate Determining Chu oxolinic acid, method is easy, reliable, rapid, highly sensitive, reappearance and specificity good.
Description
Technical field
The invention belongs to medication chemistry technical field of quality detection, particularly a kind of Ce Dings the liquid phase chromatography analytical method of oxolinic acid content.
Background technology
Oxolinic acid is also known as Yang Huan oxolinic acid, OA, Olympic acid (Oxilinic acid), english abbreviation OA, the second generation product of quinolones, for white band yellow-white column crystallization or crystalline powder, odorless, tasteless, fusing point 320 DEG C, water-soluble and ethanol hardly, can be dissolved in formic acid and sodium hydroxide solution, nonhygroscopic, to heat, wet, light is more stable.It has stronger broad spectrum activity, stronger antibacterial efficacy is had to Gram-negative bacteria and a part of positive bacteria, and with microbiotic without cross resistance, but antibacterial action is not had to fungi and tubercle bacillus, there is consumption low, the advantages such as good antimicrobial effect, external aquaculturist thinks that it treats one of ideal medicine of aquatic animal disease, to Vibrio anguillarum, has great antibacterial activity addicted to fish-pathogenic bacterias such as aqueous vapor pseudomonas bacillus.
In the import veterinary medical quality standard of current enforcement and European Pharmacopoeia, the assay of oxolinic acid all adopts non-aqueous titration to measure, because chemical synthesis is prepared in oxolinic acid containing a small amount of acid impurities, the colour developing of acid base indicator can be disturbed, and the existence of acid impurities, can cause measurement result than actual higher.
In addition, although disclose the method that some adopt Ye phase chromatography Ce oxolinic acid content in existing document, but its measurement range is little, be applicable to the measurement of Di Han Liang oxolinic acid, be not suitable for measuring chemical synthesis and prepare oxolinic acid product content and measurement result is undesirable.As existing document discloses a kind of detection technique research of aquatic products Zhong oxolinic acid residual quantity; Particularly, liquid phase chromatography is adopted to measure, high-efficient liquid phase chromatogram condition is that chromatographic column adopts anti-phase C18 post, fluorescence detector excitation wavelength is 325nm, emission wavelength is 369nm, mobile phase is 0.02mol/L phosphoric acid+acetonitrile+tetrahydrofuran (volume ratio is 69: 16: 15), and flow velocity is 0.8ml/min.The oxolinic acid typical curve range of linearity is at 10 ~ 200ng/mL.Under variable concentrations level, the recovery of oxolinic acid is 79% ~ 93%, and the coefficient of variation is less than 10%, detects and is limited to 10 μ g/kg.
Summary of the invention
The object of the invention is to the deficiency making up above-mentioned prior art, provide a kind of Ce and Ding liquid chromatography (HPLC) analytical approach of oxolinic acid content, adopt the method to be effectively separated with impurity A, B, C by Shi oxolinic acid, the true Ce of Zhun Dings the content of oxolinic acid product.Described technical scheme is as follows: embodiments provide a kind of Ce and Ding the liquid phase chromatography analytical method of oxolinic acid content, the method comprises the following steps: the preparation of (1) testing sample solution: be dissolved in 75-85 DEG C (heating water bath) in the mixed solvent of dimethyl formamide and methyl alcohol 2:3 ~ 5 by volume by Dai Ce oxolinic acid sample, be mixed with the solution that concentration is 0.1 ~ 0.5mg/mL, obtain sample solution with the filtering with microporous membrane of 0.22 μm ~ 0.45 μm.
(2) sample detection: the content of the sample solution Zhong oxolinic acid adopting external standard method step (1) to obtain, its chromatographic condition is: chromatographic column is C18 post, mobile phase: acetonitrile, the organic modifiers adding organic base (number percent that organic base accounts for mobile phase cumulative volume is 0.02-0.05%) and the water adding organic acid (number percent that organic acid accounts for mobile phase cumulative volume is 0.2-0.5%) are the mixed solution that 10 ~ 30:5 ~ 20:60 ~ 90 form by volume, flow velocity: 0.3 ~ 1.2mL/min, determined wavelength: 300 ~ 350nm, column temperature: 35 ~ 45 DEG C, sample size: 5 ~ 20 μ L.Wherein, organic base comprises three n-hexylamines, three positive heptyl amice or tri-n-octyl amines etc., and organic modifiers comprises methyl alcohol or tetrahydrofuran etc., and organic acid comprises acetic acid, trifluoroacetic acid or citric acid etc.
Preferably, in abovementioned steps (1), the volume ratio of dimethyl formamide and methyl alcohol is 2:3.
Preferably, in abovementioned steps (1), sample dissolution temperature is 80 DEG C.
Wherein, in abovementioned steps (2), the chromatographic column of C18 post to be Stationary liquid be octadecyl silane, column length 150 ~ 250mm × internal diameter 4.6mm × packing material size 3 ~ 10 μm.
Preferably, in abovementioned steps (2), organic modifiers is tetrahydrofuran.
Preferably, in abovementioned steps (2), organic base is tri-n-octyl amine.
Preferably, in abovementioned steps (2), organic acid is citric acid.
Preferably, in abovementioned steps (2), the volume ratio of acetonitrile, the organic modifiers adding organic base and interpolation organic acid water is 20:10:70.
Wherein, in abovementioned steps (2), the number percent that organic base accounts for mobile phase cumulative volume is 0.03%.
Wherein, in abovementioned steps (2), the number percent that organic acid accounts for mobile phase cumulative volume is 0.3%.
Preferably, in abovementioned steps (2), the flow velocity of mobile phase is 0.5mL/min, and determined wavelength is 330nm, and column temperature is 40 DEG C.
Particularly, the Ce that the embodiment of the present invention provides Dings the liquid phase chromatography analytical method of oxolinic acid content, comprise: the preparation of (1) testing sample solution and reference substance solution: get Shi Liang oxolinic acid sample, after dissolving in 80 DEG C of water-baths in the mixed solvent of dimethyl formamide and methyl alcohol 2:3 ~ 5 by volume, be mixed with the solution that concentration is 0.1 ~ 0.5mg/mL, with the filtering with microporous membrane of 0.22 μm ~ 0.45 μm; Qu oxolinic acid reference substance is appropriate, with method preparation, for stratographic analysis.
(2) sample detection: adopt octadecyl silane to be the chromatographic column of Stationary liquid, column length 150 ~ 250mm × internal diameter 4.6mm × packing material size 3 ~ 10 μm, mobile phase is by acetonitrile, the organic solvent adding organic base (number percent accounting for mobile phase cumulative volume is 0.03%) and the water adding organic acid (number percent accounting for mobile phase cumulative volume is 0.3%) are the mixed solution that 10 ~ 30:5 ~ 20:60 ~ 90 form by volume, flow velocity is 0.3 ~ 1.2mL/min, determined wavelength is 300 ~ 350nm, column temperature is 35 ~ 45 DEG C, get testing sample solution that step (1) prepares and reference substance solution injects high performance liquid chromatograph, sample size is 5 ~ 20 μ L, spectrogram is obtained after detection.
(3) cubage: adopt external standard method to calculate the content of testing sample Zhong oxolinic acid according to the spectrogram that step (2) obtains.
As shown from the above technical solution, the present invention is the chromatographic column utilizing octadecyl silane to be Stationary liquid, adopts liquid phase chromatography Shi oxolinic acid to be effectively separated with each impurity, thus the content of Accurate Determining Yang Pin Zhong oxolinic acid.Result with optimal conditions shows that ， oxolinic acid has good linear relationship within the scope of 0.05mg/mL ~ 2.5mg/mL, and RSD is 1.66%.Measuring method provided by the invention is easy, reliable, rapid, highly sensitive, favorable reproducibility, and specificity is good, is suitable for the mensuration of Dui oxolinic acid product content.
Accompanying drawing explanation
Fig. 1 is the chromatogram of sample in embodiment 1 Zhong oxolinic acid assay, and its main peak appearance time is 17.575min, and impurity A appearance time is 11.386min, and impurity B appearance time is 13.010min, and impurity C appearance time is 15.475min;
Fig. 2 is the chromatogram of reference substance in embodiment 1 Zhong oxolinic acid assay, and its main peak appearance time is 17.541min.
Embodiment
Below by way of specific embodiment, the present invention is further illustrated, but protection content of the present invention is not limited to following examples.
In following examples instrument and reagent as follows: Shimadzu Lc20A high performance liquid chromatograph, UV-detector, LC-solution chromatographic work station; Octadecyl silane is the chromatographic column (column length 150 ~ 250mm × internal diameter 4.6mm × packing material size 3 ~ 10 μm) of Stationary liquid, electronic analytical balance, water-bath.Oxolinic acid reference substance is produced by Sigma company, and content is 98.0% ， oxolinic acid sample is Masteam Bio-tech Co., Ltd.'s self-control; Acetonitrile, tetrahydrofuran, tri-n-octyl amine are import chromatographically pure, and dimethyl formamide, citric acid are that domestic analysis is pure.
Embodiment 1
Octadecyl silane is adopted to be the chromatographic column of Stationary liquid, column length 150mm × internal diameter 4.6mm × packing material size 5 μm, mobile phase is acetonitrile: tetrahydrofuran (tri-n-octyl amine containing accounting for mobile phase cumulative volume 0.03%): water (citric acid containing accounting for mobile phase cumulative volume 0.3%)=20:10:70, flow velocity is 0.5mL/min, determined wavelength is 330nm, column temperature is 40 DEG C, and sample size is 10 μ L.Precision takes 20mg oxolinic acid sample (lot number 130801) and reference substance respectively, to in 100mL volumetric flask, add the mixed solvent (volume ratio is 2:3) of appropriate dimethyl formamide and methyl alcohol, after dissolving in 80 DEG C of water-baths, the mixed solvent adding above-mentioned dimethyl formamide and methyl alcohol is again diluted to scale, with the filtering with microporous membrane of 0.45 μm before sample introduction, for stratographic analysis.
Get above-mentioned sample solution and reference substance solution, respectively injecting chromatograph, record 25min detection time, obtain chromatogram, as depicted in figs. 1 and 2, by external standard method Suan oxolinic acid content, Ce oxolinic acid sample size is 97.8% to its chromatogram.
Embodiment 2
Octadecyl silane is adopted to be the chromatographic column of Stationary liquid, column length 150mm × internal diameter 4.6mm × packing material size 10 μm, mobile phase is acetonitrile: tetrahydrofuran (tri-n-octyl amine containing accounting for mobile phase cumulative volume 0.04%): water (citric acid containing accounting for mobile phase cumulative volume 0.3%)=20:10:70, flow velocity is 0.45mL/min, determined wavelength is 320nm, column temperature is 35 DEG C, and sample size is 10 μ L.Precision takes 20mg oxolinic acid sample (lot number 130802) and reference substance respectively, to in 100mL volumetric flask, add the mixed solvent (volume ratio is 2:3) of appropriate dimethyl formamide and methyl alcohol, after dissolving in 78 DEG C of water-baths, the mixed solvent adding above-mentioned dimethyl formamide and methyl alcohol is again diluted to scale, with the filtering with microporous membrane of 0.45 μm before sample introduction, for stratographic analysis.
Get above-mentioned sample solution and reference substance solution, respectively injecting chromatograph, record 25min detection time, obtain chromatogram, by external standard method Suan oxolinic acid content, Ce oxolinic acid sample size is 97.6%.
Embodiment 3
Octadecyl silane is adopted to be the chromatographic column of Stationary liquid, column length 150mm × internal diameter 4.6mm × packing material size 5 μm, mobile phase is acetonitrile: tetrahydrofuran (tri-n-octyl amine containing accounting for mobile phase cumulative volume 0.03%): water (citric acid containing accounting for mobile phase cumulative volume 0.4%)=20:10:70, flow velocity is 0.55mL/min, determined wavelength is 310nm, column temperature is 40 DEG C, and sample size is 20 μ L.Precision takes 20mg oxolinic acid sample (lot number 130803) and reference substance respectively, to in 100mL volumetric flask, add the mixed solvent (volume ratio is 2:3) of appropriate dimethyl formamide and methyl alcohol, after dissolving in 80 DEG C of water-baths, the mixed solvent adding above-mentioned dimethyl formamide and methyl alcohol is again diluted to scale, with the filtering with microporous membrane of 0.22 μm before sample introduction, for stratographic analysis.
Get above-mentioned sample solution and reference substance solution, respectively injecting chromatograph, record 25min detection time, obtain chromatogram, by external standard method Suan oxolinic acid content, Ce oxolinic acid sample size is 97.9%.
Embodiment 4
Octadecyl silane is adopted to be the chromatographic column of Stationary liquid, column length 250mm × internal diameter 4.6mm × packing material size 5 μm, mobile phase is acetonitrile: tetrahydrofuran (tri-n-octyl amine containing accounting for mobile phase cumulative volume 0.05%): water (citric acid containing accounting for mobile phase cumulative volume 0.5%)=20:10:70, flow velocity is 0.55mL/min, determined wavelength is 310nm, column temperature is 40 DEG C, and sample size is 20 μ L.Precision takes 20mg oxolinic acid sample (lot number 130804) and reference substance respectively, to in 100mL volumetric flask, add the mixed solvent (volume ratio is 1:2) of appropriate dimethyl formamide and methyl alcohol, after dissolving in 80 DEG C of water-baths, the mixed solvent adding above-mentioned dimethyl formamide and methyl alcohol is again diluted to scale, with the filtering with microporous membrane of 0.45 μm before sample introduction, for stratographic analysis.
Get above-mentioned sample solution and reference substance solution, respectively injecting chromatograph, record 35min detection time, obtain chromatogram, by external standard method Suan oxolinic acid content, Ce oxolinic acid sample size is 97.5%.
Embodiment 5
Octadecyl silane is adopted to be the chromatographic column of Stationary liquid, column length 250mm × internal diameter 4.6mm × packing material size 5 μm, mobile phase is acetonitrile: tetrahydrofuran (tri-n-octyl amine containing accounting for mobile phase cumulative volume 0.05%): water (citric acid containing accounting for mobile phase cumulative volume 0.5%)=15:15:75, flow velocity is 0.55mL/min, determined wavelength is 310nm, column temperature is 5 DEG C, and sample size is 20 μ L.Precision takes 20mg oxolinic acid sample (lot number 130805) and reference substance respectively, to in 100mL volumetric flask, add the mixed solvent (volume ratio is 2:3) of appropriate dimethyl formamide and methyl alcohol, after dissolving in 80 DEG C of water-baths, the mixed solvent adding above-mentioned dimethyl formamide and methyl alcohol is again diluted to scale, with the filtering with microporous membrane of 0.45 μm before sample introduction, for stratographic analysis.
Get above-mentioned sample solution and reference substance solution, respectively injecting chromatograph, record 35min detection time, obtain chromatogram, by external standard method Suan oxolinic acid content, Ce oxolinic acid sample size is 97.1%.
Embodiment 6 couples of Ce of the present invention Ding the methodological study of oxolinic acid sample size.
1. specificity
Precision takes 20mg oxolinic acid sample (lot number 130801), to in 100mL volumetric flask, add the mixed solvent (volume ratio is 2:3) of appropriate dimethyl formamide and methyl alcohol, after dissolving in 80 DEG C of water-baths, the mixed solvent adding above-mentioned dimethyl formamide and methyl alcohol is again diluted to scale, with after the membrane filtration of 0.45 μm before sample introduction, detect by the chromatographic condition of embodiment 1, sample size is 10 μ L.Result display impurity A, impurity B can be separated Yu oxolinic acid completely with impurity C, and degree of separation is respectively 4.33,4.96,3.79, and its chromatogram as shown in Figure 1.
2. linear relationship is investigated
Accurate Cheng Qu oxolinic acid sample (lot number 130801) is appropriate, be mixed with concentration with the mixed solvent (volume ratio is 2:3) of dimethyl formamide and methyl alcohol and be respectively 0.05mg/mL, 0.1 mg/mL, 0.2 mg/mL, 0.4 mg/mL, 0.8 mg/mL, 1.5 mg/mL, 2.5 mg/mL oxolinic acid solution, after the membrane filtration of 0.45 μm, peak area is measured according to the chromatographic condition sample introduction in embodiment 1, peak area is respectively 339253, 743089, 1508724, 3053281, 6123356, 11803124, 18910342, take sample concentration as horizontal ordinate, peak area is ordinate, drawing standard curve, calculating regression equation is Y=8 × 10
6x+14883, there is good linear relationship correlation coefficient r=0.9997 within the scope of 0.05 ~ 2.5 mg/mL, and RSD is 1.66%.
3. stability test
Take 20mg oxolinic acid sample (lot number 130801), according to the method in embodiment 1 and chromatographic condition, prepare sample solution and detect, respectively 0,1,2,4,8,12,24h sample introduction, the peak area of sample introduction 7 Ji Lu oxolinic acids altogether, its peak area coefficient of variation is that 1.62%, Biao Ming oxolinic acid solution is stable in 24h.
4. the precision test of chromatographic system
Take 20mg oxolinic acid sample (lot number 130801), according to the method in embodiment 1 and chromatographic condition, prepare sample solution and detect, continuous sample introduction 5 times, the peak area of note record oxolinic acid, its coefficient of variation is 0.78%, shows that chromatographic system precision is good.
5. method replica test
Precision takes 20mg oxolinic acid sample (lot number 130801), totally 5 parts, according to the method in embodiment 1 and chromatographic condition, prepare sample solution and detect, continuous sample introduction 5 times, the peak area of note record oxolinic acid, its coefficient of variation is 1.65%, shows that the method repeatability is good.
Verify through test of many times, showing to adopt octadecyl silane of the present invention to be the chromatographic column of Stationary liquid and mobile phase is acetonitrile: tetrahydrofuran (containing 0.03% tri-n-octyl amine): water (containing 0.3% citric acid)=20:10:70, in 25 minutes, oxolinic acid can effectively be separated with impurity A, impurity B, impurity C, and peak shape is sharp-pointed, repeatability is good, therefore the assay of this invention Shi Yong Yu oxolinic acid.Certainly, under other chromatographic conditions provided by the invention, effect is desirable equally, and the present invention omits detailed description.
In sum, the present invention Dui oxolinic acid and impurity A, impurity B, impurity C Xia same chromatographic condition are effectively separated, and adopt Standard reference Dui oxolinic acid content to measure, and method is simple, fast, accurately, are that Ce Dings the Perfected process of oxolinic acid content.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. survey and determine the liquid phase chromatography analytical method of oxolinic acid content, described method with in dividing from oxolinic acid and impurity A, B, C, is characterized in that, said method comprising the steps of:
(1) preparation of testing sample solution: Dai Ce oxolinic acid sample is dissolved in the mixed solvent of dimethyl formamide and methyl alcohol 2:3 ~ 5 by volume in 75-85 DEG C, be mixed with the solution that concentration is 0.1 ~ 0.5mg/mL, obtain sample solution with the filtering with microporous membrane of 0.22 μm ~ 0.45 μm;
(2) sample detection: the content adopting sample solution Zhong oxolinic acid described in external standard method, its chromatographic condition is: chromatographic column is C18 post, mobile phase: acetonitrile, the organic modifiers adding organic base and interpolation organic acid water are the mixed solution that 10 ~ 30:5 ~ 20:60 ~ 90 form by volume, flow velocity: 0.3 ~ 1.2mL/min, determined wavelength: 300 ~ 350nm, column temperature: 35 ~ 45 DEG C, sample size: 5 ~ 20 μ L, described organic base is tri-n-octyl amine, described organic modifiers comprises methyl alcohol or tetrahydrofuran, and described organic acid is citric acid.
2. Ce according to claim 1 Dings the liquid phase chromatography analytical method of oxolinic acid content, and it is characterized in that: in step (1), the volume ratio of described dimethyl formamide and methyl alcohol is 2:3.
3. the liquid phase chromatography analytical method of oxolinic acid content is Dinged according to the Ce described in claim 1, it is characterized in that: in step (2), the chromatographic column of described C18 post to be Stationary liquid be octadecyl silane, column length 150 ~ 250mm × internal diameter 4.6mm × packing material size 3 ~ 10 μm.
4. Ce according to claim 1 Dings the liquid phase chromatography analytical method of oxolinic acid content, and it is characterized in that: in step (2), described organic modifiers is tetrahydrofuran.
5. the liquid phase chromatography analytical method of oxolinic acid content is determined in survey according to claim 1, it is characterized in that: in step (2), and the volume ratio of described acetonitrile, the organic modifiers adding organic base and interpolation organic acid water is 20:10:70.
6. Ding the liquid phase chromatography analytical method of oxolinic acid content according to the Ce described in claim 1, it is characterized in that: in step (2), the number percent that described organic base accounts for mobile phase cumulative volume is 0.03%.
7. Ding the liquid phase chromatography analytical method of oxolinic acid content according to the Ce described in claim 1, it is characterized in that: in step (2), the number percent that described organic acid accounts for mobile phase cumulative volume is 0.3%.
8. the Ce according to any one of claim 1-7 Dings the liquid phase chromatography analytical method of oxolinic acid content, and it is characterized in that: in step (2), the flow velocity of described mobile phase is 0.5mL/min, and described determined wavelength is 330nm, and described column temperature is 40 DEG C.
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Non-Patent Citations (5)
| Title |
|---|
| Herve´Pouliquen等.Rapid and simple determination of oxolinic acid and oxytetracycline in the shell of the blue mussel (Mytilus edulis) by high-performance liquid chromatography.《JOURNAL OF CHROMATOGRAPHY B》.1997,第702卷157-162. * |
| High-performance liquid chromatographic determination of oxolinic acid and flumequine in the live fish feed Artemia;Maria Touraki等;《JOURNAL OF CHROMATOGRAPHY B》;20011231;第751卷;247-256 * |
| 检测鸡蛋中12 种喹诺酮类药物残留的HPLC方法;廖兰等;《中国农业科学》;20081231;第41卷(第8期);2419-2424 * |
| 高效液相色谱法测定水产品中的恶喹酸;郭德华等;《化学分析计量》;20031231;第12卷(第1期);24-25 * |
| 鸡蛋和牛奶中噁喹酸、氟甲喹残留的检测方法研究;李倩等;《中国兽药杂志》;20121231;第46卷(第8期);文章摘要、第1-2节 * |
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