CN115166094A - Method for detecting toltrazuril content - Google Patents
Method for detecting toltrazuril content Download PDFInfo
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- CN115166094A CN115166094A CN202210838082.1A CN202210838082A CN115166094A CN 115166094 A CN115166094 A CN 115166094A CN 202210838082 A CN202210838082 A CN 202210838082A CN 115166094 A CN115166094 A CN 115166094A
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- acetonitrile
- solution
- mobile phase
- toltrazuril
- detecting
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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
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/70—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in livestock or poultry
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention provides a method for detecting the content of toltrazuril, which comprises the following steps: preparing a test solution: taking a proper amount of sample, precisely weighing, placing in a volumetric flask, diluting to a scale with a mobile phase, shaking up, performing ultrasonic treatment, cooling to room temperature, filtering, and precisely measuring a subsequent filtrate to be used as a test solution; (2) setting a reference substance solution: taking a proper amount (about 50 mg) of a reference substance, precisely weighing, and diluting to scale in a 100ml volumetric flask by flowing to obtain a reference substance solution; (3) carrying out high performance liquid chromatography analysis: a chromatographic column: selecting octadecylsilane bonded silica gel column; mobile phase: the potassium dihydrogen phosphate acetonitrile oil is prepared by mixing potassium dihydrogen phosphate and acetonitrile in a volume ratio of: acetonitrile =50:50. the invention optimizes the preparation ratio of the mobile phase to be 1, simplifies the preparation, simultaneously replaces acetonitrile-water solution with the mobile phase to optimize the complicated operation when preparing the reference solution and the sample solution and optimizes the detection wavelength to be 240nm.
Description
Technical Field
The invention relates to the field of drug analysis, in particular to a method for detecting toltrazuril content.
Background
Coccidiosis in livestock and poultry is a protozoal disease caused by Eimeria or Eimeria necatrix parasitizing in the intestinal tract or bile duct epithelial cells of a host. The disease is distributed worldwide, the damage to livestock and poultry cultivated intensively in the world is serious, and great economic loss is caused to the livestock and poultry industry. Economic losses are mainly caused by diarrhea, weight loss, growth retardation and daily gain loss of animals. Nowadays, the prevention and treatment of coccidiosis have good effect, the phenomenon of high mortality rate caused by coccidiosis in the breeding industry is not very common, but the production performance is poor due to coccidian infection, and the economic loss is still huge. The effective prevention and treatment technology for coccidiosis is the key point in the research of coccidiosis at home and abroad at present, and the drug prevention and treatment is still the main means for preventing and treating coccidiosis at present. Toltrazuril is a highly effective anticoccidial drug, and has wide action parts on coccidia and has effects on two asexual cycles of coccidia, such as inhibiting schizont, nuclear division of gametophyte and wall forming body of gametophyte. The product has coccidiostat effect because it interferes with coccidian nucleus division and mitochondrial synthesis, affects respiratory and metabolic functions of the body, and can enlarge endoplasmic reticulum of cells to cause severe vacuolation.
The traditional method for detecting the content of toltrazuril is complicated, has more steps and poorer operability, and has complex process of preparing a reference substance solution and a sample solution by utilizing a mobile phase and complex process of preparing the mobile phase by self.
Disclosure of Invention
In order to solve the defects of the prior art, the method for detecting the content of toltrazuril is provided, and comprises the following steps:
1. a method for detecting the content of toltrazuril is characterized by comprising the following steps:
s1, preparing a test solution: taking a proper amount of sample, precisely weighing, placing in a volumetric flask, diluting to a scale with a mobile phase, shaking up, performing ultrasonic treatment, cooling to room temperature, filtering, and precisely measuring a subsequent filtrate to be used as a test solution;
s2, setting a reference solution: an appropriate amount (about 50 mg) of the control substance is precisely weighed and diluted to the scale by flowing in a 100ml volumetric flask to be used as the control substance solution.
S3, performing high performance liquid chromatography analysis: a chromatographic column: selecting octadecylsilane chemically bonded silica gel column;
mobile phase: the potassium dihydrogen phosphate acetonitrile oil is prepared by mixing potassium dihydrogen phosphate and acetonitrile, wherein the volume ratio is as follows: acetonitrile =1:1;
flow rate: 0.5-1.5ml/min;
ultraviolet detector wavelength: 240nm;
column temperature: 20-30 ℃;
sample introduction volume: 5-15 μ L.
Preferably, the pH of the potassium dihydrogen phosphate in S3 is 3.0.
The preferred flow rate in S3 is 1ml/min, the injection volume is 10. Mu.L, and the column temperature is 25 ℃.
Has the advantages that:
(1) Different from the traditional method for detecting the toltrazuril content, the method adopts a common liquid chromatograph, has low requirements on instruments and has strong operability.
(2) The method for detecting the content of toltrazuril optimizes the preparation proportion of the mobile phase as 1:1, simplifying the configuration process of the mobile phase; meanwhile, the invention uses the mobile phase to replace acetonitrile-water solution, thus simplifying the complicated operation of preparing the reference solution and the sample solution.
(3) The method for detecting the content of toltrazuril provided by the invention determines the optimal detection wavelength to be 240nm through optimization.
Detailed Description
For the purpose of enhancing understanding of the present invention, the present invention will be further described in detail with reference to the following examples, which are provided for illustration only and are not to be construed as limiting the scope of the present invention.
A method for detecting the content of toltrazuril comprises the following steps:
s1, preparing a test solution: taking 50mg of sample, precisely weighing, placing in a 100ml volumetric flask, diluting to a scale with a mobile phase, shaking up, performing ultrasonic treatment for 10 minutes, cooling to room temperature, and filtering, wherein 10 mu L of subsequent filtrate is precisely measured to be used as a test solution;
s2, setting a reference solution: an appropriate amount (about 50 mg) of the control substance is precisely weighed and diluted to the scale by flowing in a 100ml volumetric flask to be used as the control substance solution.
S3, performing high performance liquid chromatography analysis: a chromatographic column: selecting octadecylsilane chemically bonded silica gel column;
mobile phase: the potassium dihydrogen phosphate acetonitrile oil is prepared by mixing potassium dihydrogen phosphate and acetonitrile in a volume ratio of: acetonitrile =1:1;
flow rate: 1ml/min;
ultraviolet detector wavelength: 240nm;
column temperature: 25 ℃;
sample injection volume: 10 μ L.
The invention adopts a common liquid chromatograph, has low requirements on the instrument and has strong operability. Optimizing the preparation ratio of the mobile phase to 1:1, simplifying the configuration process of the mobile phase; meanwhile, the mobile phase is used for replacing acetonitrile-water solution, so that the complex operation of preparing reference solution and sample solution is simplified; through optimization, the optimal detection wavelength is determined to be 240nm.
As a further improvement, the above-mentioned is only a preferred embodiment of the present invention, and should not be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. A method for detecting the content of toltrazuril is characterized by comprising the following steps:
s1, preparing a test solution: taking a proper amount of sample, precisely weighing, placing in a volumetric flask, diluting to a scale with a mobile phase, shaking up, ultrasonically treating, cooling to room temperature, filtering, and precisely measuring subsequent filtrate as a test solution;
s2, setting a reference substance solution: an appropriate amount (about 50 mg) of the control substance is precisely weighed and diluted to the scale by flowing in a 100ml volumetric flask to be used as the control substance solution.
S3, performing high performance liquid chromatography analysis: and (3) chromatographic column: selecting octadecylsilane bonded silica gel column;
mobile phase: the potassium dihydrogen phosphate acetonitrile oil is prepared by mixing potassium dihydrogen phosphate and acetonitrile, wherein the volume ratio is as follows: acetonitrile =1:1;
flow rate: 0.5-1.5ml/min;
ultraviolet detector wavelength: 240nm;
column temperature: 20-30 ℃;
sample introduction volume: 5-15 μ L.
2. The method for detecting the content of toltrazuril according to claim 1, wherein the pH of the potassium dihydrogen phosphate in S3 is 3.0.
3. The method for detecting the content of toltrazuril according to claim 1, wherein the flow rate in S3 is 1ml/min, the injection volume is 10 μ L, and the column temperature is 25 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210838082.1A CN115166094A (en) | 2022-07-18 | 2022-07-18 | Method for detecting toltrazuril content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210838082.1A CN115166094A (en) | 2022-07-18 | 2022-07-18 | Method for detecting toltrazuril content |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115166094A true CN115166094A (en) | 2022-10-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210838082.1A Pending CN115166094A (en) | 2022-07-18 | 2022-07-18 | Method for detecting toltrazuril content |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009121957A1 (en) * | 2008-04-03 | 2009-10-08 | Krka, Tovarna Zdravil, D.D., Novo Mesto | Toltrazuril with improved dissolution properties |
| CN103271921A (en) * | 2013-05-10 | 2013-09-04 | 华南农业大学 | Preparation method of compound solution of toltrazuril and diclazuril and application thereof |
| CN104374840A (en) * | 2014-10-31 | 2015-02-25 | 广东新峰药业股份有限公司 | Method for measuring content of chlorpheniramine maleate in chlorpheniramine maleate cream by high-performance liquid chromatography |
| CN111024848A (en) * | 2019-12-25 | 2020-04-17 | 镇江益生堂水产生物有限公司 | Separation tube for preparing samples for detecting toltrazuril content in blood and detection method |
| CN113640411A (en) * | 2021-07-30 | 2021-11-12 | 海南海神同洲制药有限公司 | Method for detecting related substances of clindamycin phosphate vaginal tablets |
| CN114113397A (en) * | 2021-11-30 | 2022-03-01 | 江苏知原药业股份有限公司 | Content determination method for active ingredients of pirfenidone tablets |
-
2022
- 2022-07-18 CN CN202210838082.1A patent/CN115166094A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009121957A1 (en) * | 2008-04-03 | 2009-10-08 | Krka, Tovarna Zdravil, D.D., Novo Mesto | Toltrazuril with improved dissolution properties |
| CN103271921A (en) * | 2013-05-10 | 2013-09-04 | 华南农业大学 | Preparation method of compound solution of toltrazuril and diclazuril and application thereof |
| CN104374840A (en) * | 2014-10-31 | 2015-02-25 | 广东新峰药业股份有限公司 | Method for measuring content of chlorpheniramine maleate in chlorpheniramine maleate cream by high-performance liquid chromatography |
| CN111024848A (en) * | 2019-12-25 | 2020-04-17 | 镇江益生堂水产生物有限公司 | Separation tube for preparing samples for detecting toltrazuril content in blood and detection method |
| CN113640411A (en) * | 2021-07-30 | 2021-11-12 | 海南海神同洲制药有限公司 | Method for detecting related substances of clindamycin phosphate vaginal tablets |
| CN114113397A (en) * | 2021-11-30 | 2022-03-01 | 江苏知原药业股份有限公司 | Content determination method for active ingredients of pirfenidone tablets |
Non-Patent Citations (1)
| Title |
|---|
| 张志美;邓旭明;沈志强;: "HPLC对妥曲珠利纳米乳中有效成分含量的检测", 动物医学进展, no. 06, pages 521 * |
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