CN103776936A - Method for determining content of ivermectin, albendazole sulfoxide and praziquantel in tetramizole - Google Patents
Method for determining content of ivermectin, albendazole sulfoxide and praziquantel in tetramizole Download PDFInfo
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- CN103776936A CN103776936A CN201410065084.7A CN201410065084A CN103776936A CN 103776936 A CN103776936 A CN 103776936A CN 201410065084 A CN201410065084 A CN 201410065084A CN 103776936 A CN103776936 A CN 103776936A
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- ivermectin
- praziquantel
- methyl alcohol
- albendazole
- acetonitrile
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Abstract
The invention discloses a method for determining content of ivermectin, albendazole sulfoxide and praziquantel in tetramizole. A mobile phase is methanol-acetonitrile-water (volume ratio of 30-50-10), the flow rate is 1.2ml/min, a chromatographic column is C18(4.6*250mm 5microns), the column temperature is 25 DEG C, a thinner is methanol, the sampling size is 20mu l, and the detection wavelength is 245nm. The contents of the ivermectin, the albendazole sulfoxide and the praziquantel in the tetramizole are detected by adopting the high-performance liquid method disclosed by the invention, and the method has the advantages of being short in sample analysis time, low in detection cost, high in accuracy and precision, wide in effective detection range and the like.
Description
Technical field
The present invention relates to a kind of efficient liquid-phase chromatography method of measuring ivermectin, albendazole, praziquantel content in pest-resistant medicine for animals " tetramisole ".
Background technology
Parasitic disease is the common disease of animal.Various parasites can cause animal poor appetite or useless absolutely, gastricism, become thin, vomiting, anaemia, the symptom such as be obstructed of growing.Because domestic animal frequently contacts with parasite every day, greatly increase ill probability.Parasite consumes Animal nutrition, reduces the price of deed, reduces production performance, strengthens aquaculture cost, and the economic loss causing is huge often.Domestic animal has parasite parasitism.In the time that polypide infective dose is few, carcass is not fallen ill, but can make breast, meat, hair output reduce, and physique declines, and while butchering, trunk and internal organ are discarded, other viral or bacteriosises of secondary etc. when weak.In the time that polypide infective dose is larger, livestock nutrition is extremely low, also can cause large quantities of death.China's livestock and poultry total amount accounts for prostatitis, the world, and the economic loss that verminosis of animal causes is huge.Conventional anthelmintic is short action time, and expelling parasite spectrum is narrow, needs repeated multiple times medication.Therefore, development and application long-acting insect expelling preparation, can reduce the polypide load of livestock and poultry greatly, thereby improves the economic benefit of aquaculture.
The research of long-acting, broad-spectrum anthelmintic formulation necessitates, and ivermectin is the semi-synthetic macrolides polycomponent broad-spectrum anti-parasite medicine producing from soil microorganism A Foman streptomycete fermentation.Ivermectin has good repelling and killing efficacy to endoparasite and ectoparasite and arthropod, and ivermectin is difficult for seeing through blood-brain barrier, and livestock is had to higher security.Albendazole, by affecting the multiple biochemical metabolism approach of polypide, can be killed rapidly the worm in body.Praziquantel is pyrazine isoquinilone derivatives, for broad-spectrum anti-parasite medicine, especially blood fluke is had to killing action.Praziquantel has the features such as curative effect is high, toxicity is low, spinoff is light, short treating period, wide accommodation.
Tetramisole is that ivermectin, albendazole, praziquantel, synergistic agent and sustained release agent etc. are made to compound preparation, expanding most possibly expelling parasite composes to adapt to livestock and poultry parasite and prevents and treats the actual needs of process, adopt modern medicines novel formulation technique this product to be made slow-release injected simultaneously, extend curative effect, thoroughly kill all kinds of parasites in livestock and poultry inside and outside.
Summary of the invention
The present invention seeks to set up the method for tetramisole quality control, measure the high performance liquid chromatography of ivermectin in tetramisole, albendazole, praziquantel content simultaneously.Specifically implement by following technical method:
A kind of method that the invention provides ivermectin, albendazole, praziquantel in high effective liquid chromatography for measuring tetramisole, it selects octadecyl silane chromatographic column, and take methyl alcohol-acetonitrile-water as mobile phase, detection wavelength is 245nm.
The length of chromatographic column is 150mm-250mm, selects 150mm chromatographic column, and preferable flow rate is 0.8ml/min, selects 250mm chromatographic column, and preferable flow rate is 1.2ml/min.Mobile phase is methyl alcohol-acetonitrile-water, and methyl alcohol volume fraction is 20 ~ 45%, and methyl alcohol volume fraction is 40 ~ 60%, and methyl alcohol preferred volume is 30%, and acetonitrile preferred volume is 50%; 20 ~ 40 ℃ of column temperatures, preferably column temperature is 25 ℃.Detect the preferred 245nm of wavelength.
Reference substance and need testing solution preparation:
It is appropriate that precision takes ivermectin, albendazole and praziquantel reference substance, adds methyl alcohol and dissolve and dilute the reference substance solution of making in every 1ml containing ivermectin 0.5mg, albendazole 0.3mg, praziquantel 0.2mg.
Precision takes tetramisole parenteral solution 1ml, puts in 100ml volumetric flask, adds methyl alcohol ultrasonic dissolution to clarification, is settled to scale, shakes up, and obtains need testing solution.
Sample determination:
Adopt auto injection method to get respectively 20 μ l reference substance and need testing solutions, by external standard method with calculated by peak area content.
Its related substances=reference substance concentration * test sample peak area/contrast peak area * 100%
Linear relationship is investigated:
Precision measures above-mentioned middle reference substance solution 0.2,0.5,1.0,2.0,5.0,10.0ml, be placed in respectively 10ml volumetric flask, add methyl alcohol and be diluted to scale, shake up, obtain the reference substance solution of 6 concentration, by preferred color of choice spectral condition, detect successively, take reference substance sample size (μ g) logarithm X as horizontal ordinate, peak area logarithm Y(mAU*s) be ordinate, drawing standard curve.The regression equation that obtains ivermectin is: Y=6751.4X+214.2, and r=0.9992, the range of linearity is 0.2 μ g ~ 10 μ g; The regression equation of albendazole is: Y=2133.7X-34.1, and r=0.9997, the range of linearity is 0.12 μ g ~ 6 μ g; The regression equation of praziquantel is: Y=16636.9X+127.8, and r=0.9996, the range of linearity is 0.08 μ g ~ 4 μ g.
Precision is investigated:
It is appropriate that precision measures reference substance solution, by preferred color of choice spectral condition, and each sample difference continuous sample introduction 6 times.The peak area RSD of reference substance ivermectin is 0.64%, and the peak area RSD of albendazole is 0.93%, and the peak area RSD of praziquantel is 0.91%
Study on the stability: reference substance is detected by preferred color of choice spectral condition respectively at 0h, 2h, 4h, 8h, 12h, 24h, the peak area of ivermectin, albendazole, praziquantel does not obviously change, RSD is respectively 0.54%, 0.43%, 0.77%, and result shows that ivermectin, albendazole, praziquantel solution are good at 24h internal stability.
Application of sample recovery test: the ivermectin, albendazole and the praziquantel sample that accurately take known content are appropriate, precision adds high concentration reference substance solution 0.8ml, 1ml, 1.2ml respectively again, 3 parts of each parallel preparations, detect by preferred color of choice spectral condition, calculate recovery rate, it is 99.76%, 100.21%, 99.51% that result ivermectin, albendazole and praziquantel average recovery rate are respectively, and RSD is 0.76%, 0.34%, 0.61%, shows that the method average recovery is good.
The present invention passes through linear relationship investigation, precision investigation, study on the stability and application of sample recovery test etc. method is verified, result shows the method accurately and reliably, detects rapidly; With low cost; Sensing range is large; Sensitivity, accuracy are high.
Accompanying drawing explanation
Fig. 1 is the structural formula of ivermectin.
Fig. 2 is the structural formula of albendazole.
Fig. 3 is the structural formula of praziquantel.
Fig. 4 is the high-efficient liquid phase chromatogram of tetramisole.
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Specific embodiment
Chromatographic condition: adopt Thermo C18,4.6 × 250mm, 5 μ m chromatographic columns; Detect wavelength 245nm; Mobile phase is methyl alcohol-acetonitrile-water (30-50-20); Flow velocity 1.2ml/min; Sample size 20 μ l; 25 ℃ of column temperatures.
Experimental procedure: it is appropriate that precision takes ivermectin, albendazole and praziquantel reference substance, adds methyl alcohol and dissolves and dilute the high concentration reference substance solution of making in every 1ml containing ivermectin 0.5mg, albendazole 0.3mg, praziquantel 0.2mg.
Precision takes tetramisole parenteral solution 1ml, puts in 100ml volumetric flask, adds methyl alcohol ultrasonic dissolution to clarification, is settled to scale, shakes up, and obtains need testing solution.
Respectively reference substance solution and need testing solution are measured as stated above in accordance with the law, recorded peak area, calculate content by external standard method.
Claims (7)
1. a method for ivermectin, albendazole and praziquantel content in high effective liquid chromatography for measuring tetramisole, is characterized in that chromatographic condition is the reverse-phase chromatographic column take octadecylsilane chemically bonded silica as filling material; Take methyl alcohol-acetonitrile-water as mobile phase; Flow velocity is 0.6 ~ 1.5ml/min, sample size 5 ~ 20 μ l.
2. method according to claim 1, is characterized in that mobile phase is methyl alcohol-acetonitrile-water, and methyl alcohol volume fraction is 20 ~ 45%, and methyl alcohol volume fraction is 40 ~ 60%, and methyl alcohol preferred volume is 30%, and acetonitrile preferred volume is 50%.
3. method according to claim 1, it is characterized in that chromatographic column is that octadecylsilane chemically bonded silica is filling material, flow rate of mobile phase is 0.6 ~ 1.5ml/min, 20 ~ 40 ℃ of column temperatures, select 150mm chromatographic column, preferable flow rate is 0.8ml/min, selects 250mm chromatographic column, and preferable flow rate is 1.2ml/min; Preferably column temperature is 25 ℃.
4. method according to claim 1, is characterized in that using UV-detector, and detection wavelength is 245nm.
5. method according to claim 1, is characterized in that thinning agent is methyl alcohol.
6. method according to claim 1, is characterized in that sample size is 5 ~ 20 μ l, and preferably sample size is 20 μ l.
7. method according to claim 1, is characterized in that in reference substance solution in every 1ml solution containing ivermectin 0.5mg, albendazole 0.3mg, praziquantel 0.2mg.
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| CN201410065084.7A CN103776936A (en) | 2014-02-26 | 2014-02-26 | Method for determining content of ivermectin, albendazole sulfoxide and praziquantel in tetramizole |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105181839A (en) * | 2015-09-06 | 2015-12-23 | 中国农业科学院兰州畜牧与兽药研究所 | Method for detecting residual quantity of ivermectin in sheep muscle tissues by using liquid chromatograph/mass spectrometer with doramectin as internal standard substance |
| CN108120782A (en) * | 2017-12-29 | 2018-06-05 | 佛山市南海东方澳龙制药有限公司 | A kind of assay method of ivermectin chewable tablets dissolution rate |
| CN111208249A (en) * | 2020-01-14 | 2020-05-29 | 信阳农林学院 | Method for determining content of effective components of anthelmintic by high performance liquid chromatography |
| CN115267011A (en) * | 2022-09-06 | 2022-11-01 | 重庆市食品药品检验检测研究院 | Liquid chromatography-mass spectrometry chromatography method for qualitative detection of illegally added drugs in oil control cosmetics |
-
2014
- 2014-02-26 CN CN201410065084.7A patent/CN103776936A/en active Pending
Non-Patent Citations (4)
| Title |
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| FLAVIA LADA DEGAUT PONTES等: "DEVELOPMENT AND VALIDATION OF AN HPLC-MS/MS METHOD FOR SIMULTANEOUS DETERMINATION OF IVERMECTIN, FEBANTEL, PRAZIQUANTEL, PYRANTEL PAMOATE AND RELATED COMPOUNDS IN FIXED DOSE COMBINATION FOR VETERINARY USE", 《ASIAN JOURNAL OF PHARMACEUTICAL AND CLINICAL RESEARCH》 * |
| K NA-BANGCHANG K等: "High-performance liquid chromatographic method for the determination of ivermectin in plasma", 《SOUTHEAST ASIAN J TROP MED PUBLIC HEALTH》 * |
| 厉文辉等: "加速溶剂萃取-高效液相色谱-串联质谱法同时检测鱼肉中喹诺酮、磺胺与大环内酯类抗生素", 《分析测试学报》 * |
| 王硕等: "超高效液相色谱_串联质谱测定污泥中氯霉素、磺胺类、喹诺酮类、四环素类与大环内酯类抗生素", 《分析测试学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105181839A (en) * | 2015-09-06 | 2015-12-23 | 中国农业科学院兰州畜牧与兽药研究所 | Method for detecting residual quantity of ivermectin in sheep muscle tissues by using liquid chromatograph/mass spectrometer with doramectin as internal standard substance |
| CN108120782A (en) * | 2017-12-29 | 2018-06-05 | 佛山市南海东方澳龙制药有限公司 | A kind of assay method of ivermectin chewable tablets dissolution rate |
| CN111208249A (en) * | 2020-01-14 | 2020-05-29 | 信阳农林学院 | Method for determining content of effective components of anthelmintic by high performance liquid chromatography |
| CN111208249B (en) * | 2020-01-14 | 2022-11-18 | 信阳农林学院 | Method for determining content of active ingredients of anthelmintic by high performance liquid chromatography |
| CN115267011A (en) * | 2022-09-06 | 2022-11-01 | 重庆市食品药品检验检测研究院 | Liquid chromatography-mass spectrometry chromatography method for qualitative detection of illegally added drugs in oil control cosmetics |
| CN115267011B (en) * | 2022-09-06 | 2024-05-07 | 重庆市食品药品检验检测研究院 | Liquid chromatography-mass spectrometry chromatography method for qualitative detection of illegally added drugs in oil-control cosmetics |
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Application publication date: 20140507 |