CN107907601A - The detection method of Marbofloxacin content in a kind of dog plasma - Google Patents
The detection method of Marbofloxacin content in a kind of dog plasma Download PDFInfo
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- CN107907601A CN107907601A CN201711012327.0A CN201711012327A CN107907601A CN 107907601 A CN107907601 A CN 107907601A CN 201711012327 A CN201711012327 A CN 201711012327A CN 107907601 A CN107907601 A CN 107907601A
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- marbofloxacin
- dog plasma
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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Abstract
The invention discloses a kind of detection method of Marbofloxacin content in dog plasma, it includes the following steps：1) the dog plasma sample containing Marbofloxacin is taken, addition Ofloxacin is internal standard, is vortexed and mixes 8~13s, then adds acetonitrile precipitation albumen, is vortexed and mixes 20~40s, stands 2~4min, supernatant is pipetted after centrifugal treating；2) supernatant obtained by step 1) is added mobile phase solution and redissolved, crossed 0.22 μm of miillpore filter, must treat test sample through 50 DEG C of dryings of nitrogen evaporator；3) take and treat test sample obtained by step 2), qualitative and quantitative detection is carried out to it by LC MS/MS methods.The present invention is using Ofloxacin as internal standard, with acetonitrile precipitation plasma protein, substantially increase the recovery rate of Marbofloxacin in dog plasma, and quantitative detection further carries out it using LC MS/MS methods, gained testing result is accurate, and detection process step is simple, specificity is high, time-consuming short, quick, accurately analysis determining method is provided for Marbofloxacin Clinical pharmacokinetics etc..
Description
Technical field
The present invention relates to the detection method in detection method field, more particularly to medicament residue.
Background technology
Marbofloxacin is fluoroquinolone antibacterial agent, dedicated for for animals.Marbofloxacin acts on the aerobic gram of wide spectrum
Negative and some gram-positive bacterias, and Mycoplasma, have height bactericidal activity.As third generation Marbofloxacin medicine, its
Also be predominantly targeting and act on duplication and transcriptase, such as DNA helicase and topoisomerase I V, both to bacteria living all very
It is important.
Marbofloxacin can be absorbed well by oral and drug administration by injection, and toxic side effect is relatively low, thus more and more
Deep and superficial skin infection, urinary tract infections applied to treatment dog.
The detection mode of Marbofloxacin in dog plasma is established, clinical rational drug use can be instructed.Horse in detection blood plasma at present
The method of ripple sand star content mainly has：Anti- high performance liquid chromatography, high performance liquid chromatography (HPLC)-fluorescence detection, fluorescence point
Light photometry, high performance capillary electrophoresis, wherein high performance liquid chromatography is most commonly used that both at home and abroad, but sensitivity is not high, detection
Time, length was, it is necessary to which sample size is larger.
Based on this, I am proposed to found a kind of detection mode of rapidly and efficiently high sensitivity.Efficient liquid phase-electron spray-series connection
Mass spectrography, test limit is low, and sensitive height, analysis time is fast, needs sample amount few, compares the development in the epoch of complying with.
The content of the invention
It is an object of the invention to for above-mentioned existing detection method sensitivity is not high, detection time is long, needs sample amount big
A kind of deficiency, there is provided the detection method of Marbofloxacin content in dog plasma.
The technical solution used in the present invention is：The detection method of Marbofloxacin content in a kind of dog plasma, it is included such as
Lower step：
1) the dog plasma sample containing Marbofloxacin is taken, addition Ofloxacin is internal standard, is vortexed and mixes 8~13s, Ran Houjia
Enter acetonitrile precipitation albumen, be vortexed and mix 20~40s, stand 2~4min, supernatant is pipetted after centrifugal treating；
2) supernatant obtained by step 1) is added mobile phase solution and redissolved, cross 0.22 μm of micropore through 50 DEG C of dryings of nitrogen evaporator
Filter membrane, must treat test sample；
3) take and treat test sample obtained by step 2), qualitative and quantitative detection is carried out to it by LC-MS/MS methods.
Further as such scheme is improved, and the concentration of Ofloxacin described in step 1) is 250 μ g/mL.Specifically,
Ofloxacin is fluoroquinolone antibacterial agent, its molecular structure is similar to Marbofloxacin, and molecular weight is close, while and Marbofloxacin
Compared to stability higher, therefore the present invention chooses Ofloxacin as internal standard, can better ensure that the accuracy of the detection method
And reappearance.
Further as such scheme is improved, and temperature control is 3~5 during the centrifugal treating described in step 1)
DEG C, centrifugal speed 12000r/min, centrifugation time 10min.Specifically, the restriction of the centrifugal treating condition can effectively improve
Precipitation and the stability of supernatant, make centrifugal effect more preferable, advantageously ensure that the accuracy of late detection.
Further as such scheme is improved, and mobile phase solution described in step 2) is 0.1% by acetonitrile and concentration
Aqueous formic acid is with volume ratio 20:80 mix.Specifically, the supernatant of the mobile phase solution and centrifugation gained has excellent
Compatibility, advantageously ensure that the accuracy of late detection.
The beneficial effects of the invention are as follows：The present invention using Ofloxacin as internal standard, with acetonitrile precipitation plasma protein, significantly
The recovery rate of Marbofloxacin in dog plasma is improved, and quantitative detection, gained inspection further carry out it using LC-MS/MS methods
It is accurate to survey result, and detection process step is simple, specificity is high, time-consuming short, is that Marbofloxacin Clinical pharmacokinetics etc. provide
Quick, accurately analysis determining method.
Brief description of the drawings
Fig. 1 a of the present invention are the ion stream chromatograms for treating Marbofloxacin in test sample；
Fig. 1 b of the present invention are the ion stream chromatograms for treating internal standard Ofloxacin in test sample.
Embodiment
The present invention is specifically described with reference to embodiment, in order to technical field personnel to the present invention
Understand.It is necessary that herein the present invention will be further described it is emphasized that embodiment is only intended to, it is impossible to be interpreted as to this
The limitation of invention protection domain, fields person skilled in the art, the non-intrinsically safe made according to foregoing invention content to the present invention
The modifications and adaptations of property, should still fall within protection scope of the present invention.Mentioned raw materials following at the same time are unspecified, are
Commercial product；The processing step or preparation method not referred in detail be processing step known to a person skilled in the art or
Preparation method.
The detection method of Marbofloxacin content in the dog plasma of the present invention, it includes the following steps：
1) the dog plasma sample containing Marbofloxacin is taken, it is internal standard to add the Ofloxacin that 50 μ L concentration are 250 μ g/mL,
It is vortexed and mixes 8~13s, then add acetonitrile precipitation albumen, be vortexed and mix 20~40s, stands 2~4min, centrifugal treating, centrifugation
Temperature control is at 3~5 DEG C, centrifugal speed 12000r/min, centrifugation time 10min in processing procedure, after pipette supernatant；
2) supernatant obtained by step 1) is added mobile phase solution and redissolved, the flowing mixes through 50 DEG C of dryings of nitrogen evaporator
Liquid is by aqueous formic acid that acetonitrile and concentration are 0.1% with volume ratio 20:80 mix, and then cross 0.22 μm of miillpore filter,
It must treat test sample；
3) take and treat test sample obtained by step 2), carry out quantitative detection to it by LC-MS/MS methods.
Specifically, the testing conditions of LC-MS/MS methods described in step 3) are as shown in table 1 below, final detection result such as attached drawing
Shown in 1a and attached drawing 1b, wherein attached drawing 1a is the ion stream chromatogram for treating Marbofloxacin in test sample, and attached drawing 1b is interior in test sample to treat
Mark the ion stream chromatogram of thing Ofloxacin.
The testing conditions of 1 LC-MS/MS methods of table
Above-described embodiment is the preferred embodiment of the present invention, all with similar technique of the invention and the equivalence changes made,
The protection category of the present invention should all be belonged to.
Claims (4)
1. the detection method of Marbofloxacin content in a kind of dog plasma, it is characterised in that include the following steps：
1) the dog plasma sample containing Marbofloxacin is taken, addition Ofloxacin is internal standard, is vortexed and mixes 8~13s, then adds second
Nitrile protein precipitation, is vortexed and mixes 20~40s, stands 2~4min, supernatant is pipetted after centrifugal treating；
2) supernatant obtained by step 1) is redissolved through 50 DEG C of dryings of nitrogen evaporator, addition mobile phase solution, crosses 0.22 μm of miillpore filter,
It must treat test sample；
3) take and treat test sample obtained by step 2), carry out quantitative detection to it by LC-MS/MS methods.
2. the detection method of Marbofloxacin content in a kind of dog plasma according to claim 1, it is characterised in that：Step 1)
Described in the concentration of Ofloxacin be 250 μ g/mL.
3. the detection method of Marbofloxacin content in a kind of dog plasma according to claim 1, it is characterised in that：Step 1)
Described in centrifugal treating during temperature control at 3~5 DEG C, centrifugal speed 12000r/min, centrifugation time 10min.
4. the detection method of Marbofloxacin content in a kind of dog plasma according to claim 1, it is characterised in that：Step 2)
Described in mobile phase solution by aqueous formic acid that acetonitrile and concentration are 0.1% with volume ratio 20:80 mix.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711012327.0A CN107907601A (en) | 2017-10-25 | 2017-10-25 | The detection method of Marbofloxacin content in a kind of dog plasma |
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| CN201711012327.0A CN107907601A (en) | 2017-10-25 | 2017-10-25 | The detection method of Marbofloxacin content in a kind of dog plasma |
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| CN201711012327.0A Pending CN107907601A (en) | 2017-10-25 | 2017-10-25 | The detection method of Marbofloxacin content in a kind of dog plasma |
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Citations (5)
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| CN101315351A (en) * | 2008-06-26 | 2008-12-03 | 江南大学 | HPLC-ESI-MS/MS measuring method for simultaneously detecting 19 kinds of carbostyril medicaments |
| CN103884790A (en) * | 2014-03-21 | 2014-06-25 | 烟台杰科检测服务有限公司 | Method for determining multiresidue of veterinary drugs in animal-derived foods |
| CN104990996A (en) * | 2015-05-19 | 2015-10-21 | 江苏出入境检验检疫局动植物与食品检测中心 | Method for detecting antibiotic residues in milk, and application thereof |
| KR20160004733A (en) * | 2014-07-04 | 2016-01-13 | 대한민국(관리부서 : 농림축산식품부 농림축산검역본부) | Method of analyzing blood marbofloxacin concentration |
| CN106124683A (en) * | 2016-08-26 | 2016-11-16 | 中国兽医药品监察所 | A kind of method of multiple antimicrobial component in veterinary drug of detection simultaneously |
-
2017
- 2017-10-25 CN CN201711012327.0A patent/CN107907601A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101315351A (en) * | 2008-06-26 | 2008-12-03 | 江南大学 | HPLC-ESI-MS/MS measuring method for simultaneously detecting 19 kinds of carbostyril medicaments |
| CN103884790A (en) * | 2014-03-21 | 2014-06-25 | 烟台杰科检测服务有限公司 | Method for determining multiresidue of veterinary drugs in animal-derived foods |
| KR20160004733A (en) * | 2014-07-04 | 2016-01-13 | 대한민국(관리부서 : 농림축산식품부 농림축산검역본부) | Method of analyzing blood marbofloxacin concentration |
| CN104990996A (en) * | 2015-05-19 | 2015-10-21 | 江苏出入境检验检疫局动植物与食品检测中心 | Method for detecting antibiotic residues in milk, and application thereof |
| CN106124683A (en) * | 2016-08-26 | 2016-11-16 | 中国兽医药品监察所 | A kind of method of multiple antimicrobial component in veterinary drug of detection simultaneously |
Non-Patent Citations (8)
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| M.A.GARCIA等: "Determination of marbofloxacin in plasma samples by high-performance liquid chromatography using fluorescence detection", 《JOURNAL OF CHROMATOGRAPHY B》 * |
| M.SCHNEIDER等: "Pharmacokinetics of marbofloxacin in dogs after oral and parenteral Administration", 《J. VET. PHARMACOL. THERAP.》 * |
| ROBL.COKE等: "PRELIMINARY SINGLE-DOSE PHARMACOKINETICS OF MARBOFLOXACIN IN BALL PYTHONS (PYTHON REGIUS)", 《JOURNAL OF ZOO AND WILD LIFE MEDICINE》 * |
| SILESHI YOHANNES等: "Pharmacokinetics and pharmacokinetic/pharmacodynamic integration of marbofloxacin after intravenous and intramuscular administration in beagle dogs", 《XENOBIOTICA》 * |
| 单奇等: "马波沙星在罗非鱼体内的药物代谢动力学研究", 《华南农业大学学报》 * |
| 卢燕等: "马波沙星在多杀性巴氏杆菌感染的小鼠体内的药动学研究", 《中国兽医科学》 * |
| 曹长福等: "肌注马波沙星在犊黄牛体内的药动学及半体内抗菌后效应研究", 《畜牧兽医学报》 * |
| 瞿颖等: "马波沙星在健康小鼠和感染多杀性巴氏杆菌小鼠体内的药动学比较", 《华南农业大学学报》 * |
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Application publication date: 20180413 |