CN102081078A - Method for measuring residual quantities of four fluoroquinolone medicaments in animal food - Google Patents
Method for measuring residual quantities of four fluoroquinolone medicaments in animal food Download PDFInfo
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Abstract
The invention discloses a method for measuring residual quantities of four fluoroquinolone medicaments in animal food, and relates to a liquid chromatography method for measuring the residual quantities of medicaments in animal food. The invention aims to provide a measuring method which is simple and quick in operation, high in automation degree, high in extraction efficiency, high in recovery rate and good in repeatability. The method for measuring the residual quantities of the four fluoroquinolone medicaments in the animal food comprises the following steps: sample preparation; sample pretreatment: accurately weighing a sample, mixing the sample and kieselguhr uniformly, transferring the mixture to an extraction tank, placing the extraction tank on a quick solvent extraction instrument to perform extraction, adding n-hexane and diethyl ether into the obtained extract to remove lipid impurities, performing violent oscillation, standing for demixing, removing the n-hexane-diethyl ether layer, repeatedly operating for two times, transferring the solution at the lower layer to a concentration bottle, rotationally steaming the solution in a rotary evaporator till the solution is dried, dissolving the dregs by using a mobile phase, and filtering the solution through a filter membrane for high performance liquid chromatography (HPLC) analysis; preparation of a standard solution; and efficient liquid chromatography measurement.
Description
Technical field
The present invention relates to a kind of assay method of animal food veterinary drug residue amount, particularly relate to a kind of assay method that is used for measuring simultaneously animal food Norfloxacin, Ciprofloxacin, Enrofloxacin, four kinds of fluo quinolone drug residual amounts of sarafloxacin.
Background technology
Fluoroquinolones belongs to the antibacterials of synthetic, is widely used in the bacteriosis of control aquatic livestock, also is usually used in the sterilization of pond and water body, also promotes growth of animal as feed addictive sometimes, improves the speed of growth and output.But this medicine will inevitably cause its residual in animal food in the extensive and a large amount of use of veterinary clinic, can the serious harm human beings'health if do not controlled; Influence the outlet of China's animal food, cause enormous economic loss.China and European Union have all formulated the maximum residue limit(MRL) of multiple fluoroquinolones in animal tissue.[in No. 1025 bulletin-14-2008 animal foods of the Ministry of Agriculture fluo quinolone drug residual detect high performance liquid chromatography] have stipulated the assay method of the fluoroquinolones in the animal food, for the detection of such residue of veterinary drug amount provides the analysis foundation.But this method is being carried out sample pre-treatments employing phosphate buffered solution homogenate vibration extraction, and centrifugal then collection supernatant, gained supernatant still need to purify with the method for Solid-Phase Extraction.Operation steps is numerous and diverse, and the time is long, can not robotization.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of simple to operate, fast, and automaticity height, extraction efficiency height, the assay method of four kinds of fluo quinolone drug residual amounts in the animal food of the recovery and good reproducibility.
The assay method of four kinds of fluo quinolone drug residual amounts in the animal food of the present invention may further comprise the steps:
A, specimen preparation: sample is rubbed freezing preservation;
B, sample pre-treatments: accurately take by weighing sample, evenly do not have to lump with zeyssatite is mixed to sample, being transferred to the bottom puts in the abstraction pool of one deck fiber filter paper, abstraction pool is positioned on the quick solvent extraction instrument extracts, add normal hexane and ether removal lipid impurity in the resulting extract, static layering behind the thermal agitation, discard normal hexane-ether layer, add twice of normal hexane and ether repetitive operation again, lower floor's solution changes over to and concentrates in the bottle, vacuum rotary steam is to doing in the Rotary Evaporators of 40 ℃ of water-baths, and with the moving phase dissolved residue, solution is analyzed for HPLC through membrane filtration;
The preparation of c, standard solution: accurately take by weighing Norfloxacin, Ciprofloxacin, Enrofloxacin, sarafloxacin standard items, it is dissolved in the 0.03mol/L sodium hydroxide solution together, be made into and contain the hybrid standard storing solution that above-mentioned four kinds of standard items and its concentration are 1mg/ml simultaneously, 2 ℃～8 ℃ keep in Dark Place, face with preceding and accurately measure above-mentioned hybrid standard storing solution, be diluted to the standard operation liquid of serial gradient with moving phase, keep in Dark Place under the cryogenic conditions, used the same day;
D, high-performance liquid chromatogram determination: draw the standard operation liquid of the variable concentrations for preparing, inject the high performance liquid chromatograph of being furnished with fluorescence detector FLD series connection UV-detector UV;
E, determination of residual amount result's calculating: carry out the qualitative analysis of fluoroquinolones with retention time, carry out the quantitative test of fluoroquinolones, use external standard method result of calculation with peak area;
The preparation of described moving phase: prepare the phosphate aqueous solution of 0.05mol/L earlier, it is transferred pH to 2.4, get 82: 18 by volume ratio of 0.05mol/L phosphoric acid solution/triethylamine, acetonitrile preparation moving phase with triethylamine.
The assay method of four kinds of fluo quinolone drug residual amounts in the animal food of the present invention, the freezing preservation condition among the wherein said step a are-18 ℃.
The assay method of four kinds of fluo quinolone drug residual amounts in the animal food of the present invention, the sample pre-treatments among the wherein said step b, the mass ratio of zeyssatite and sample is (1～3): 1; Normal hexane concentration is to add 3～5ml normal hexane in every gram sample, and ether concentration is to add 1～3ml ether in every gram sample; The solvent extraction instrument parameter is set to fast: extraction solvent: the ammoniacal liquor acetonitrile of volume parts 8%, and temperature: 80 ℃, pressure: 10.0MPa, heat time heating time: 5min, quiet hour: 5min, flush volume: 60% of abstraction pool volume, nitrogen purging time: 60s, quiet cycle number of times: 1 time; Vacuum tightness is-0.096MPa during vacuum rotary steam; The filter membrane aperture is 0.45 μ m.
The assay method of four kinds of fluo quinolone drug residual amounts in the animal food of the present invention, the standard operation liquid of serial gradient is 0.01,0.02,0.05,0.1 and 0.2mg/L among the wherein said step c.
The assay method of four kinds of fluo quinolone drug residual amounts in the animal food of the present invention, the high-efficient liquid phase chromatogram condition that adopts in the wherein said steps d is: matrix is the C18 liquid-phase chromatographic column of the ultra-pure spherical silica gel of Type B, specification is 4.6mm * 250mm * 5 μ m, silica gel purity＞99.999%, column temperature: 15～25 ℃; Flow rate of mobile phase is 0.8mL/min, and sample size is 20 μ L; The excitation wavelength of fluorescence detector is 265nm, and emission wavelength is 478nm; The UV-detector wavelength is 271nm.
The assay method of four kinds of fluo quinolone drug residual amounts in the animal food of the present invention, wherein said quick solvent extraction instrument is selected the quick solvent extraction instrument of the APLE2000 of Beijing Jitian Instrument Co., Ltd. for use.
The quick solvent extraction instrument of the assay method utilization of four kinds of fluo quinolone drug residual amounts extracts fluoroquinolones in the animal food in the animal food of the present invention under High Temperature High Pressure, extract advances high performance liquid chromatography fluorescence detector (FLD) series connection UV-detector (UV) and carries out assay determination through purifying.The solvent extraction sample pretreatment process is simple fast, whole operation automaticity height, and fluorescence detector (FLD) series connection UV-detector (UV) is measured accurate, highly sensitive, good reproducibility.
Description of drawings
Fig. 1 is Norfloxacin, Ciprofloxacin, Enrofloxacin, sarafloxacin standard items fluorescence chromatogram;
Fig. 2 is Norfloxacin, Ciprofloxacin, Enrofloxacin, sarafloxacin standard items ultraviolet chromatogram.
Embodiment
The assay method of four kinds of fluo quinolone drug residual amounts may further comprise the steps in the animal food of the present invention:
The preparation of standard solution: accurately take by weighing Norfloxacin, Ciprofloxacin, Enrofloxacin, sarafloxacin standard items, it is dissolved in the 0.03mol/L sodium hydroxide solution together, be made into and contain the hybrid standard storing solution that above-mentioned four kinds of standard items and its concentration are 1mg/ml simultaneously, 2 ℃～8 ℃ keep in Dark Place, face with preceding and accurately measure above-mentioned hybrid standard storing solution, be diluted to concentration with moving phase and be respectively 0.01,0.02,0.05,0.1 and the standard operation liquid of 0.2mg/L, keep in Dark Place under 4 ℃ of conditions, used the same day.The preparation of moving phase: prepare the phosphate aqueous solution of 0.05mol/L earlier, it is transferred pH to 2.4, get 82: 18 by volume ratio of 0.05mol/L phosphoric acid solution/triethylamine, acetonitrile preparation moving phase with triethylamine.
High-performance liquid chromatogram determination: draw the standard operation liquid of the variable concentrations for preparing, inject the high performance liquid chromatograph of being furnished with fluorescence detector FLD series connection UV-detector UV.High-efficient liquid phase chromatogram condition is: matrix is the C18 liquid-phase chromatographic column of the ultra-pure spherical silica gel of Type B, and specification is 4.6mm * 250mm * 5 μ m, silica gel purity＞99.999%, column temperature: 15 ℃; Flow rate of mobile phase is 0.8mL/min, and sample size is 20 μ L; The excitation wavelength of fluorescence detector is 265nm, and emission wavelength is 478nm; The UV-detector wavelength is 271nm.
Determination of residual amount embodiment 1:
Measure 8 whitefish samples, sample is rubbed, under-18 ℃ of conditions, store.
Sample pre-treatments: accurately take by weighing the sample after 1.0g thaws, place mortar together, be ground to sample and obviously do not lump with 1.5g zeyssatite, place the bottom to put the 11mL abstraction pool of one deck fiber filter paper in sample, extraction conditions is: the ammoniacal liquor acetonitrile of using volume parts 8% is as extracting reagent, 80 ℃ of temperature, pressure 10MPa, heating 5min, the static 5min that extracts circulates 1 time, and elution volume is 60% abstraction pool volume, get sample express developed with acetonitrile, nitrogen purging is collected whole extracts.Add 3ml normal hexane and 1ml ether removal lipid impurity in the gained extract, vibration back static layering discards normal hexane-ether layer, repetitive operation twice, lower floor's solution change over to and concentrate in the bottle vacuum rotary steam in the Rotary Evaporators of 40 ℃ of water-baths, vacuum tightness-0.096MPa is concentrated into dried.With the moving phase dissolved residue, and accurately be settled to 2mL, solution is analyzed for HPLC through 0.45 μ m membrane filtration.The solvent extraction instrument is selected the quick solvent extraction instrument of the APLE2000 of Beijing Jitian Instrument Co., Ltd. for use fast.
Determination of residual amount result's calculating: carry out the qualitative analysis of fluoroquinolones with retention time, carry out the quantitative test of fluoroquinolones with peak area, use external standard method result of calculation, the result does not all detect in 8 parts of whitefish samples and contains 4 kinds of fluo quinolone drug residuals.
Repeatability and determination of recovery rates:
Adopt negative whitefish meat sample (four kinds of fluoroquinolones all do not have detect) to measure, determine the detectability of analyte with 3 times of signal to noise ratio (S/N ratio)s, determine the quantitative limit of analyte with 10 times of signal to noise ratio (S/N ratio)s, in conjunction with the recovery and sample size, quantitatively detecting of method is limited to 4.3-10.0 μ g/kg, adopt the method for adding standard solution in the sample, under same sample preparation condition, four kinds of fluoroquinolones are carried out the recovery of standard addition experiment, the results are shown in Table 2.
Table 1 liquid phase chromatography detects the range of linearity, related coefficient, detection limit and the quantitative limit of four kinds of fluoroquinolones
The recovery of fluoroquinolones and Precision test result (n=5) in the table 2 whitefish meat
Determination of residual amount embodiment 2:
Measure 10 beef samples, sample is rubbed, under-18 ℃ of conditions, store.
Sample pre-treatments: accurately take by weighing the sample after 1.0g thaws, place mortar together, be ground to sample and obviously do not lump with 1.5g zeyssatite, place the bottom to put the 11mL abstraction pool of one deck fiber filter paper in sample, extraction conditions is: the ammoniacal liquor acetonitrile of using volume parts 8% is as extracting reagent, 80 ℃ of temperature, pressure 10MPa, heating 5min, the static 5min that extracts circulates 1 time, and elution volume is 60% abstraction pool volume, get sample express developed with acetonitrile, nitrogen purging is collected whole extracts.Add 3ml normal hexane and 1ml ether removal lipid impurity in the gained extract, vibration back static layering discards normal hexane-ether layer, repetitive operation twice, lower floor's solution change over to and concentrate in the bottle vacuum rotary steam in the Rotary Evaporators of 40 ℃ of water-baths, vacuum tightness-0.096MPa is concentrated into dried.With the moving phase dissolved residue, and accurately be settled to 2mL, solution is analyzed for HPLC through 0.45 μ m membrane filtration.The solvent extraction instrument is selected the quick solvent extraction instrument of the APLE2000 of Beijing Jitian Instrument Co., Ltd. for use fast.
Determination of residual amount result's calculating: carry out the qualitative analysis of fluoroquinolones with retention time, carry out the quantitative test of fluoroquinolones with peak area, use external standard method result of calculation, the result detects in 1 part of beef sample and contains Ciprofloxacin 105 μ g/kg, and other beef samples do not detect fluo quinolone drug residual.
Repeatability and determination of recovery rates:
Adopt negative beef sample (four kinds of fluoroquinolones all do not have detect) to measure, adopt the method for adding standard solution in the sample, under same sample preparation condition, four kinds of fluoroquinolones are carried out the recovery of standard addition experiment, the results are shown in Table 3.
The recovery of fluoroquinolones and Precision test result (n=5) in table 3 beef
Above-described embodiment is described preferred implementation of the present invention; be not that scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that those of ordinary skills make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (6)
1. the assay method of four kinds of fluo quinolone drug residual amounts in the animal food may further comprise the steps:
A, specimen preparation: sample is rubbed freezing preservation;
B, sample pre-treatments: accurately take by weighing sample, evenly do not have to lump with zeyssatite is mixed to sample, being transferred to the bottom puts in the abstraction pool of one deck fiber filter paper, abstraction pool is positioned on the quick solvent extraction instrument extracts, add normal hexane and ether removal lipid impurity in the resulting extract, static layering behind the thermal agitation, discard normal hexane-ether layer, add twice of normal hexane and ether repetitive operation again, lower floor's solution changes over to and concentrates in the bottle, vacuum rotary steam is to doing in the Rotary Evaporators of 40 ℃ of water-baths, and with the moving phase dissolved residue, solution is analyzed for HPLC through membrane filtration;
The preparation of c, standard solution: accurately take by weighing Norfloxacin, Ciprofloxacin, Enrofloxacin, sarafloxacin standard items, it is dissolved in the 0.03mol/L sodium hydroxide solution together, be made into and contain the hybrid standard storing solution that above-mentioned four kinds of standard items and its concentration are 1mg/ml simultaneously, 2 ℃～8 ℃ keep in Dark Place, face with preceding and accurately measure above-mentioned hybrid standard storing solution, be diluted to the standard operation liquid of serial gradient with moving phase, keep in Dark Place under the cryogenic conditions, used the same day;
D, high-performance liquid chromatogram determination: draw the standard operation liquid of the variable concentrations for preparing, inject the high performance liquid chromatograph of being furnished with fluorescence detector FLD series connection UV-detector UV;
E, determination of residual amount result's calculating: carry out the qualitative analysis of fluoroquinolones with retention time, carry out the quantitative test of fluoroquinolones, use external standard method result of calculation with peak area;
The preparation of described moving phase: prepare the phosphate aqueous solution of 0.05mol/L earlier, it is transferred pH to 2.4, get 82: 18 by volume ratio of 0.05mol/L phosphoric acid solution/triethylamine, acetonitrile preparation moving phase with triethylamine.
2. the assay method of four kinds of fluo quinolone drug residual amounts in the animal food according to claim 1 is characterized in that: the freezing preservation condition among the described step a is-18 ℃.
3. the assay method of four kinds of fluo quinolone drug residual amounts in the animal food according to claim 1 is characterized in that: the sample pre-treatments among the described step b, the mass ratio of zeyssatite and sample are (1～3): 1; Normal hexane concentration is to add 3～5ml normal hexane in every gram sample, and ether concentration is to add 1～3ml ether in every gram sample; The solvent extraction instrument parameter is set to fast: extraction solvent: the ammoniacal liquor acetonitrile of volume parts 8%, and temperature: 80 ℃, pressure: 10.0MPa, heat time heating time: 5min, quiet hour: 5min, flush volume: 60% of abstraction pool volume, nitrogen purging time: 60s, quiet cycle number of times: 1 time; Vacuum tightness is-0.096MPa during vacuum rotary steam; The filter membrane aperture is 0.45 μ m.
4. the assay method of four kinds of fluo quinolone drug residual amounts in the animal food according to claim 1 is characterized in that: the standard operation liquid of serial gradient is 0.01,0.02,0.05,0.1 and 0.2mg/L among the described step c.
5. the assay method of four kinds of fluo quinolone drug residual amounts in the animal food according to claim 1, it is characterized in that: the high-efficient liquid phase chromatogram condition that adopts in the described steps d is: matrix is the C18 liquid-phase chromatographic column of the ultra-pure spherical silica gel of Type B, specification is 4.6mm * 250mm * 5 μ m, silica gel purity＞99.999%, column temperature: 15～25 ℃; Flow rate of mobile phase is 0.8mL/min, and sample size is 20 μ L; The excitation wavelength of fluorescence detector is 265nm, and emission wavelength is 478nm; The UV-detector wavelength is 271nm.
6. according to the assay method of four kinds of fluo quinolone drug residual amounts in one of the described animal food of claim 1 to 5, it is characterized in that: described quick solvent extraction instrument is selected the quick solvent extraction instrument of the APLE2000 of Beijing Jitian Instrument Co., Ltd. for use.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104316615A (en) * | 2014-11-01 | 2015-01-28 | 威海出入境检验检疫局检验检疫技术中心 | Method for determinating seven kinds of quinolone residues in animal-source food through membrane dialysis-high performance liquid chromatography and tandem mass spectrometry |
| CN106383180A (en) * | 2016-08-19 | 2017-02-08 | 中华人民共和国日照出入境检验检疫局 | A method of detecting a plurality of pesticide residues in silkworm pupae |
| CN107688010A (en) * | 2017-06-28 | 2018-02-13 | 昆明理工大学 | Method based on magnetic Nano material purification carbon quantum dot fluorescence sensitivity detection FQNS |
| CN109856295A (en) * | 2019-03-25 | 2019-06-07 | 东南大学 | A kind of method of fluoroquinolones residue of veterinary drug in extraction animal derived food |
| CN110221008A (en) * | 2019-06-25 | 2019-09-10 | 华中农业大学 | A method of Danofloxacin mesylate in detection Swine plasma and alveolar fluid |
| CN112611749A (en) * | 2020-10-30 | 2021-04-06 | 重庆金美新材料科技有限公司 | Method for detecting content of ammonium citrate in liquid |
| CN113406330A (en) * | 2021-06-30 | 2021-09-17 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Kit for detecting norfloxacin and detection method |
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2011
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104316615A (en) * | 2014-11-01 | 2015-01-28 | 威海出入境检验检疫局检验检疫技术中心 | Method for determinating seven kinds of quinolone residues in animal-source food through membrane dialysis-high performance liquid chromatography and tandem mass spectrometry |
| CN106383180A (en) * | 2016-08-19 | 2017-02-08 | 中华人民共和国日照出入境检验检疫局 | A method of detecting a plurality of pesticide residues in silkworm pupae |
| CN107688010A (en) * | 2017-06-28 | 2018-02-13 | 昆明理工大学 | Method based on magnetic Nano material purification carbon quantum dot fluorescence sensitivity detection FQNS |
| CN107688010B (en) * | 2017-06-28 | 2019-12-03 | 昆明理工大学 | A method of detection fluoroquinolones |
| CN109856295A (en) * | 2019-03-25 | 2019-06-07 | 东南大学 | A kind of method of fluoroquinolones residue of veterinary drug in extraction animal derived food |
| CN109856295B (en) * | 2019-03-25 | 2022-04-26 | 东南大学 | Method for extracting fluoroquinolone veterinary drug residues in animal derived food |
| CN110221008A (en) * | 2019-06-25 | 2019-09-10 | 华中农业大学 | A method of Danofloxacin mesylate in detection Swine plasma and alveolar fluid |
| CN112611749A (en) * | 2020-10-30 | 2021-04-06 | 重庆金美新材料科技有限公司 | Method for detecting content of ammonium citrate in liquid |
| CN113406330A (en) * | 2021-06-30 | 2021-09-17 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Kit for detecting norfloxacin and detection method |
| CN113406330B (en) * | 2021-06-30 | 2024-01-02 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Kit for detecting norfloxacin and detection method |
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Application publication date: 20110601 |