CN106908560A - The detection method of quinolones medicament relict in a kind of veterinary drug - Google Patents
The detection method of quinolones medicament relict in a kind of veterinary drug Download PDFInfo
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Abstract
The invention provides a kind of detection method of quinolones medicament relict in veterinary drug.Quinolones medicament relict of the present invention in LC-MS/MS veterinary drug, first standard working solution and sample solution setting liquid chromatography-tandem mass spectrometry under the conditions of sample introduction, with the presence or absence of corresponding measured object, it is necessary to meet following condition in judgement sample：The mass chromatography peak retention time occurred in sample solution is consistent with mixed-matrix standard working solution, tolerance is less than ± 2.5%, medicine corresponding to the chromatographic peak is consistent in the relative ion abundance of the relative abundance of the setting mass spectrometry ion extraction standard working solution suitable with concentration, relative abundance deviation then can determine that and contain the medicine no more than the regulation of setting.Eliminate purification process during the inventive method sample pre-treatments, it is simple with processing routine, quickly, determine accuracy rate it is high the features such as；It is analyzed from veterinary drug source, effective guarantee aquaculture drug safety, improves Animal Food Security.
Description
Technical field
The present invention relates to a kind of detection side of quinolones medicament relict in technical field of analytical chemistry, especially veterinary drug
Method.
Background technology
Quinolone (4-quinolones), is that a class is artificial synthesized also known as quinolones, pyridonecarboxylic acids or pyridine Mek-Tol Unit
The basic structure of quinolone containing 4-, there is the antiseptic of Selective depression to DNA of bacteria helicase.Due to quinolone neither micro-
Bio secretion thing is not again the analog of microorganism secretion thing, so strictly speaking it is artificial synthesized antiseptic
(Antibacterial)。
Carbostyril antibiotic is the general medicine of a class people and animals.Because it has has a broad antifungal spectrum, antibacterial activity strong and other
Antibacterials are widely used in the aquacultures such as herding, aquatic products without cross resistance and the features such as small toxic and side effect, are included in
It is used for disease prevention and cure in the cultivation of chicken, duck, goose, pig, ox, sheep, fish, shrimp, crab etc..Because QNS is in animal body group
Residual in knitting, carbostyril antibiotic just remains accumulation in human body after people's edible animal tissue, causes human body diseases to this
The serious drug resistance of medicine, influences the treatment of human body diseases.Mankind animal of the long-term consumption containing low concentration QNS
The transmission of the property easy in-ductive drug -tolerance of food, so as to influence the clinical efficacy of such medicine.Therefore, quinolones medicament relict is asked
Topic increasingly causes the concern of people.FAO (Food and Agriculture Organization of the United Nation)/joint the committee of World Health Organization food additives expert, Europe
Alliance has all formulated MRL of various QNSs in animal tissue.U.S. FDA was announced to prohibit in 2005
Only for treating the sale of the antibacterials Enrofloxacin of poultry bacterial infection and using.China also defined ring third in 2002
7 kinds of QNSs such as Sha Xing, single promise sand star, Enrofloxacin, sarafloxacin, Difloxacin, oxolinic acid and flumequine are dynamic
MRL in thing musculature is 10~500 μ g/kg.
The content of the invention
The technical problems to be solved by the invention are the detection method for providing quinolones medicament relict in a kind of veterinary drug.
In order to solve the above technical problems, the technical scheme is that：
The detection method of quinolones medicament relict in a kind of veterinary drug, with LC-MS/MS veterinary drug
Quinolones medicament relict, comprise the following steps that：
(1) standard working solution and the sample solution sample introduction under the conditions of the liquid chromatography-tandem mass spectrometry of setting, with mass concentration
X is abscissa, and the ratio Y of peak area is ordinate, draws 5 standard working curves, the standard working solution be Ofloxacin,
Norfloxacin, 4 kinds of QNS hybrid working liquid of Ciprofloxacin and Enrofloxacin；
Sample is quantified with standard working curve, the response of medicine should be in the linear of instrument detection in sample solution
In the range of, wherein, set liquid chromatography-tandem mass spectrometry condition is as follows：
1. liquid phase chromatogram condition
Chromatographic column：Hypersil Gold C18,100mm×2.1mm,1.9μm
Mobile phase：0.1% formic acid/methyl alcohol；Flow velocity：0.35mL/min column temperatures：35 DEG C of μ L of sample size 10
Liquid phase gradient condition
2. Mass Spectrometry Conditions
Ion gun：H-ESI sources scan mode：Anion is scanned；
Detection mode：Many reaction detection spray voltages：3500V
Atomization temperature：400 DEG C of sheath atmospheric pressures：35arb
Auxiliary atmospheric pressure：10arb capillary temperatures：350℃
Four kinds of chromatographic retentions and qualitative, quantitative ion parameters of QNS
(2) under above-mentioned chromatographic condition, with the presence or absence of corresponding measured object, it is necessary to meet following condition in judgement sample：
In sample solution occur mass chromatography peak retention time it is consistent with mixed-matrix standard working solution, it is allowed to deviation be less than ±
2.5%, the medicine corresponding to the chromatographic peak is in the relative abundance of the setting mass spectrometry ion extraction standard work suitable with concentration
The relative ion abundance for making liquid is consistent, and relative abundance deviation then can determine that and contain the medicine no more than the regulation of setting.
The method for drafting of 5 standard working curves is as follows：The QNS of 100ng/mL is taken out from refrigerator
Hybrid standard working solution, recover to after room temperature with 0.1% formic acid be diluted to concentration series be 0.5ng/ml, 1ng/ml, 2ng/ml,
The standard working solution of 4ng/ml, 8ng/ml, each pin of concentration sample introduction 3 is ordinate by its gained peak area ratio average Y,
Corresponding standard concentration X is that abscissa draws standard curve.
The detection method of quinolones medicament relict in above-mentioned veterinary drug, the preparation method of the sample solution is sample warp
2% formic acid acetonitrile is extracted, and nitrogen is redissolved after blowing with 0.1% formic acid, crosses 0.22 μm of miillpore filter, and reagent is chromatogram pure reagent.
The detection method of quinolone medicine residual, the preparation method of the sample solution in above-mentioned veterinary drug, specific steps are such as
Under：
(1) 1g samples accurately are weighed, is accurate to 0.01g, be placed in 50mL polystyrene centrifuge tubes, plus the formic acid of 5mL 2%
Acetonitrile, whirling motion 1-3min, centrifugal force 4000g-6000g are centrifuged 10min under room temperature condition, extract supernatant 1ml, 55-60 DEG C of nitrogen
It is blown to do, is redissolved with 1mL0.1% formic acid, 10 times are diluted with 0.1% formic acid again after redissolution, final solution crosses 0.22 μm of micropore
Filter membrane, you can determined for liquid chromatography-tandem mass spectrometry instrument.
The beneficial effects of the invention are as follows：
The detection method of quinolone medicine residual in above-mentioned veterinary drug, with LC-MS/MS veterinary drug
Quinolones medicament relict, purification process is eliminated during the method sample pre-treatments, simple with processing routine, quickly, is determined
The features such as accuracy rate is high；It is analyzed from veterinary drug source, effective guarantee aquaculture drug safety, improves Animal Food Security.
Brief description of the drawings
Fig. 1 is that veterinary drug negative sample detects QNS (four planting sand stars) total ion current figure；
Fig. 2 be veterinary drug sample add QNS (four planting sand stars) afterwards total ion current figure (drug concentration be 1 μ g/
kg)。
Specific embodiment
In order that those skilled in the art is better understood from technical scheme, with reference to specific embodiment
Technical scheme of the present invention is described in further detail.
Embodiment 1
First, extract
The addition recovery experiment that 4 kinds of different veterinary drug samples of selection do 3 kinds of various concentrations carries out method validation, is treated in veterinary drug
The Extraction solvent of medicine is surveyed, acetonitrile, 2% formic acid acetonitrile, methyl alcohol and ethyl acetate is respectively adopted, 4 kinds of reagents carry out extraction conditions
Selection.Test result indicate that, for the quinolones residue of veterinary drug in veterinary drug, the extraction efficiency of 2% formic acid acetonitrile is better than separately
Outer two kinds of reagents.
Concrete operations：1g samples accurately are weighed, 0.01g is accurate to, is placed in 50mL polystyrene centrifuge tubes, plus 5mL
2% formic acid acetonitrile, whirling motion 1-3min, centrifugal force 4000g-6000g are centrifuged 10min under room temperature condition, extract supernatant 1ml,
55-60 DEG C of nitrogen is blown to do, and is redissolved with 1mL0.1% formic acid, and 10 times, final solution mistake are diluted with 0.1% formic acid again after redissolution
0.22 μm of miillpore filter, you can determined for liquid chromatography-tandem mass spectrometry instrument.
2nd, determine
This experiment quantitative approach is quantified by external standard method.Take out the four planting sand star medicines mixing of 100ng/mL respectively from refrigerator
Standard working solution, with recover to after room temperature with 0.1% formic acid be diluted to concentration series be 0.5ng/ml, 1ng/ml, 2ng/ml,
The standard working solution of 4ng/ml, 8ng/ml, each pin of concentration sample introduction 3 is ordinate by its gained peak area ratio average Y,
Corresponding standard concentration X is that abscissa draws standard curve.According to the medicament contg of measured object in sample, response phase is chosen
Near pharmaceutical standards working solution is analyzed simultaneously.The response of medicine all should be linear in instrument in standard working solution and prepare liquid
In response range.The curve ranges if content is above standard, are diluted to suitable dense using matrix blank solution (0.1% formic acid)
Degree post analysis.
1. liquid phase chromatogram condition
Chromatographic column：Hypersil Gold C18,100mm×2.1mm,1.9μm
Mobile phase：0.1% formic acid/methyl alcohol；Flow velocity：0.35mL/min column temperatures：35 DEG C of μ L of sample size 10
Liquid phase gradient condition
2. Mass Spectrometry Conditions
Ion gun：H-ESI sources scan mode：Anion is scanned；
Detection mode：Many reaction detection spray voltages：3500V
Atomization temperature：400 DEG C of sheath atmospheric pressures：35arb
Auxiliary atmospheric pressure：10arb capillary temperatures：350℃
Four kinds of chromatographic retentions and qualitative, quantitative ion parameters of QNS
Under above-mentioned chromatographic condition, with the presence or absence of corresponding measured object, it is necessary to meet following condition in judgement sample：Sample
The mass chromatography peak retention time occurred in solution is consistent with mixed-matrix standard working solution, it is allowed to which deviation is less than ± 2.5%, should
The phase of medicine corresponding to chromatographic peak in the relative abundance of the setting mass spectrometry ion extraction standard working solution suitable with concentration
Consistent to abundance of ions, relative abundance deviation then can determine that and contain the medicine (institute as shown in Figure 1, Figure 2 no more than the regulation of setting
Show).
3rd, case result is embodied
This experiment chooses 4 kinds of veterinary drugs and carries out QNS and does addition recovery test altogether, the curvilinear equation of its standard, returns
Yield and precision result such as following table：
The calibration curve equation and coefficient correlation of 1 four kinds of QNSs of table
The amoxicillin soluble powder determination of recovery rates result of table 2
The erythromycin thiocyanate soluble powder determination of recovery rates result of table 3
The tilmicosin solution determination of recovery rates result of table 4
The solution of diclazuril determination of recovery rates result of table 5
The amoxicillin soluble powder precision measurement result of table 6
The erythromycin thiocyanate soluble powder precision measurement result of table 7
The tilmicosin solution precision measurement result of table 8
The solution of diclazuril precision measurement result of table 9
From above case, the present invention is using the QNS in LC-MS/MS veterinary drug
Residual, the preparation method of the sample solution is sample first by water-soluble filtering, and 2% formic acid acetonitrile extraction, nitrogen is used after blowing
0.1% formic acid redissolves, and crosses 0.22 μm of miillpore filter, is then measured with Liquid Chromatography-Tandem Mass Spectrometry, appearance standard measure,
The rate of recovery is 62.3%~95.3%；With batch interior relative standard deviation 10% or so between sample batch.In sample extraction and LC-
When MS/MS is detected, treatment is all optimized to sample extracting solution and testing conditions.Detection method sample treatment journey of the invention
Sequence is simple, quick, eliminates sample purification process, reduces testing cost, and can fast and accurately determine residual in veterinary drug
The QNS for staying.It is 50 μ g/kg that method determines the lowest limit, fully meets the requirement of medicament residue detection.
It is above-mentioned with reference to specific embodiment the detection method of quinolones medicament relict in a kind of veterinary drug is carried out it is detailed
Thin description, is illustrative rather than limited, can include several embodiments according to limited scope, therefore do not taking off
Changing and modifications under present general inventive concept, should belong within protection scope of the present invention.
Claims (4)
1. in a kind of veterinary drug quinolones medicament relict detection method, it is characterised in that：Surveyed with Liquid Chromatography-Tandem Mass Spectrometry
Determine the quinolones medicament relict in veterinary drug, comprise the following steps that：
(1) standard working solution and the sample solution sample introduction under the conditions of the liquid chromatography-tandem mass spectrometry of setting, be with mass concentration X
Abscissa, the ratio Y of peak area is ordinate, draws 5 standard working curves, and the standard working solution is Ofloxacin, promise
Flucloxacillin, 4 kinds of QNS hybrid working liquid of Ciprofloxacin and Enrofloxacin；
Sample is quantified with standard working curve, the response of medicine should be in the range of linearity of instrument detection in sample solution
It is interior, wherein, set liquid chromatography-tandem mass spectrometry condition is as follows：
1. liquid phase chromatogram condition
Chromatographic column：Hypersil Gold C18,100mm×2.1mm,1.9μm
Mobile phase：0.1% formic acid/methyl alcohol；Flow velocity：0.35mL/min column temperatures：35℃
The μ L of sample size 10
Liquid phase gradient condition
2. Mass Spectrometry Conditions
Four kinds of chromatographic retentions and qualitative, quantitative ion parameters of QNS
(2) under above-mentioned chromatographic condition, with the presence or absence of corresponding measured object, it is necessary to meet following condition in judgement sample：Sample
The mass chromatography peak retention time occurred in solution is consistent with mixed-matrix standard working solution, it is allowed to which deviation is less than ± 2.5%, should
The phase of medicine corresponding to chromatographic peak in the relative abundance of the setting mass spectrometry ion extraction standard working solution suitable with concentration
Consistent to abundance of ions, relative abundance deviation then can determine that and contain the medicine no more than the regulation of setting.
2. in veterinary drug according to claim 1 quinolones medicament relict detection method, it is characterised in that：Described 5 points
The method for drafting of standard working curve is as follows：The QNS hybrid standard working solution of 100ng/mL is taken out from refrigerator,
It is 0.5ng/ml, 1ng/ml, 2ng/ml, 4ng/ml, 8ng/ml to recover to be diluted to concentration series with 0.1% formic acid to room temperature
Standard working solution, each pin of concentration sample introduction 3 is ordinate, corresponding standard concentration by its gained peak area ratio average Y
X is that abscissa draws standard curve.
3. in veterinary drug according to claim 1 quinolones medicament relict detection method, it is characterised in that：The sample
The preparation method of solution is as follows：Sample is extracted by 2% formic acid acetonitrile, and nitrogen is redissolved after blowing with 0.1% formic acid, crosses 0.22 μm of micropore
Filter membrane, reagent is chromatogram pure reagent.
4. in veterinary drug according to claim 3 quinolones medicament relict detection method, it is characterised in that：The sample
The preparation method of solution is as follows：1g samples accurately are weighed, 0.01g is accurate to, is placed in 50mL polystyrene centrifuge tubes, plus 5mL
2% formic acid acetonitrile, whirling motion 1-3min, centrifugal force 4000g-6000g are centrifuged 10min under room temperature condition, extract supernatant 1ml,
55-60 DEG C of nitrogen is blown to do, and is redissolved with 1mL0.1% formic acid, and 10 times, final solution mistake are diluted with 0.1% formic acid again after redissolution
0.22 μm of miillpore filter, you can determined for liquid chromatography-tandem mass spectrometry instrument.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108693288A (en) * | 2018-05-25 | 2018-10-23 | 无锡微色谱生物科技有限公司 | A method of quinolone drugs is extracted and analyzed using DPX pipette tips formula dispersed solid phase microextraction columns |
| CN111157649A (en) * | 2020-01-06 | 2020-05-15 | 山东省兽药质量检验所（山东省畜产品质量检测中心） | UPLC-MS/MS detection method for adding multiple medicines in scutellaria detoxification powder |
| CN113866335A (en) * | 2021-09-23 | 2021-12-31 | 南京市产品质量监督检验院 | Method for determining 81 veterinary drug residues in animal tissues by using tandem liquid chromatography-mass spectrometry and application |
| CN115586278A (en) * | 2022-10-21 | 2023-01-10 | 石家庄海关技术中心 | Detection method for quinolone drug residues in veterinary drug preparation |
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| CN113866335A (en) * | 2021-09-23 | 2021-12-31 | 南京市产品质量监督检验院 | Method for determining 81 veterinary drug residues in animal tissues by using tandem liquid chromatography-mass spectrometry and application |
| CN115586278A (en) * | 2022-10-21 | 2023-01-10 | 石家庄海关技术中心 | Detection method for quinolone drug residues in veterinary drug preparation |
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Application publication date: 20170630 |