CN109060993A - The detection method of azithromycin residual quantity in a kind of animal hair - Google Patents
The detection method of azithromycin residual quantity in a kind of animal hair Download PDFInfo
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Abstract
The invention belongs to medicament residue detection technique fields, and in particular to the detection method of azithromycin residual quantity in a kind of animal hair.This method, without livestock and poultry such as slaughter chicken, pig, oxen, realizes livestock and poultry In vivo detection using animal hair as test object；Hair sample is compared with muscle, liver, the acquisitions such as excrement are convenient, and since growth cycle of hair is long, more it can accurately monitor whether growth of animals or poultry process uses azithromycin, to realize that the food safety productions such as livestock and poultry supervise purpose, situations such as testing result is accurate, is not in false positive, false negative, high sensitivity.
Description
Technical field
The invention belongs to medicament residue detection technique fields, and in particular to azithromycin residual quantity in a kind of animal hair
Detection method.
Background technique
Azithromycin (azithromycin, AZM) is macrolide antibiotics of new generation, by the conjunction for inhibiting protein
At working, clinically it is used for the prevention of the upper lower respiratory tract of people, the urinary tract, skin and soft tissue infection and sexually transmitted disease and controls
It treats.It is concerned due to it has the characteristics that has a broad antifungal spectrum, long half time, stablizes in acidic environment, China place veterinary drug mark
Standard once included the medicine for 2004, and the Ministry of Agriculture will then be included in disabling veterinary drug list in the end of the year 2005.
Azithromycin is used for livestock and poultry cultivation in violation of rules and regulations, will affect livestock and poultry pestilence prevention and treatment and animal products safety, increase bacterium produce
The risk of raw drug resistance threatens human health.Although country prohibites, cultivating link can bring economic benefit impaired, because
This raiser will antibiotic be added into feed or used by other approach, be still abused so as to cause people with antibiotic in
Livestock and poultry become the new hidden danger for threatening animal products safety.
Domestic and foreign scholars have carried out the detection technique research of azithromycin in fraction matrix, but not yet promulgate any matrix
In the examination criteria in relation to azithromycin.Studying more detection method has in uv detection method, fluorescence detection and isotope
Mark method, but the method for using UV detector, it is extremely low to absorb weak sensitivity；Using the method for fluorescence detector, need to derive,
Measurement is time-consuming；And use Internal standard, the detection of high performance liquid chromatography-tandem mass method, method quickly, easy, specificity
By force, high sensitivity is a kind of detection method for comparing high praise in current research.
Currently, the matrix that azithromycin detects in animal products is mainly muscle, liver, blood and excrement, and muscle and
Liver needs slaughter living animal to obtain, and livestock and poultry blood sample needs professional to obtain, and needs cold chain to protect before detection
It deposits, prevents from going bad；Excrement vulnerable to pollution, sampling are also inconvenient.In addition, the medicament residue in these matrix is difficult after the off-drug period
In being detected.And hair is because of its constituent feature and lower metabolic activity, so that drug is metabolized slowly after entering,
Reservation can be accumulated for a long time, livestock and poultry hair hair in have the more long residual time, and hair sampling, convenient transportation, compared to muscle,
Liver, blood and excrement matrix be more suitable for detection sample be security of fowl product production in forbidden drug supervise provide it is more reliable
Confirm foundation.Have not yet to see azithromycin residues detection method in livestock and poultry hair.
Summary of the invention
Therefore, the technical problem to be solved in the present invention is that azithromycin in animal products in the prior art is overcome to detect
As a result unreliable, it is unfavorable for animal products security control, test sample is not easy to obtain or is difficult to the defects of saving, to provide one kind
The detection method of azithromycin residual quantity in animal hair.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
The detection method of azithromycin residual quantity in a kind of animal hair, comprising the following steps:
1. the preparation of test solution
It takes hair sample in two layers of hospital gauze, cleans, shred, mix with azithromycin-D3 working solution, be then added
Formic acid and methanol mixed solution, room temperature 30~60min of ultrasound obtain hair extracting solution, filter, drying, acetate buffer dissolution
Residue, poly- divinylbenzene sulfonic acid-vinyl pyrrolidone (MCX) modify Fe3O4Nano material magnetic solid phase extraction, ammoniated methanol are washed
It is de-, drying, with 1mL methanol aqueous solution (1:1, v/v) dissolved residue, filter membrane, as test solution；
2. high performance liquid chromatography-tandem mass method detects
High-efficient liquid phase chromatogram condition: chromatographic column: C18,2.1mm × 100mm, 1.8 μm；Mobile phase A is that volumetric concentration is
0.1% aqueous formic acid, Mobile phase B are methanol, flow velocity: 0.4mL/min；Column temperature: 35 DEG C；Sample volume: 10 μ L；Gradient elution journey
Sequence: 0~2min, 2%B linear change to 40%B；2~3min keeps 40%B, 3~4min, 40%B linear change to 75%
B；4-5min keeps 75%B, 5~5.1min, 75%B linear change to 98%B；5.1-6min keeping 98%B；6-
6.1min98% is reduced to 2%B；6.1~7.0min maintains 2%B；
Mass Spectrometry Conditions: electric spray ion source, cation scan pattern；More reaction detections: spray voltage: 3000V, ion source
Temperature, 150 DEG C, sheath temperature degree: 300 DEG C；Sheath throughput: 12L/min.
Preferably, volumetric concentration is 2~4% to the formic acid in methyl alcohol with formic acid in methanol mixed solution.
Preferably, also contain hydrogen peroxide in the methanol and formic acid mixed solution, the volume fraction of hydrogen peroxide is
0.1%~0.5%.
Preferably, the pH of the acetate buffer is 4.0~5.0, and concentration is in 0.1~0.2mol/L, with animal hair
Dosage on the basis of, the dosage of acetate buffer is in 15-40mL/g.
Preferably, the poly- divinylbenzene sulfonic acid-vinyl pyrrolidone (MCX) modifies Fe3O4Nano material dosage is
20.0~100.0mg, preparation method are, by FeCl3And FeSO4It is dissolved in the water by 2:1 (molar ratio), is passed through nitrogen protection
20min~30min, by the every mM of poly- divinylbenzene sulfonic acid of 0.05~0.2g of addition-vinyl pyrrolidone (MCX), heating
To 80 DEG C, it is rapidly added ammonium hydroxide, continues to stir 30min~60min, is alternately cleaned with secondary water and ethyl alcohol, magnet separation, gained
Nano material freeze-drying is spare.
Preferably, volume fraction is 2.0~5.0% to ammonium hydroxide in methyl alcohol in the ammoniated methanol, dosage 2.0~
5.0mL。
Preferably, on the basis of the dosage of animal hair, the dosage of the methanol and formic acid mixed solution is 40~60mL/
G, the dosage of the azithromycin-D3 working solution are 20~100 μ L/g, the concentration of azithromycin-D3 working solution is 0.5~
4.0mg/L。
Preferably, the quota ion of azithromycin is m/z749.5 > 591.4 in the Mass Spectrometry Conditions, and qualitative ion is m/
The quota ion of z749.5 > 158 and azithromycin-D3 are m/z752.4 > 594.4.
Residual quantity of the present invention according to internal standard method with calculated by peak area azithromycin in hair, calculation formula are as follows:
Azithromycin residual quantity in X-- sample, unit are ng/kg (μ g/kg)；
The concentration of c-- azithromycin standard working solution, unit are micro- gram per liter (μ g/L)；
csi-- the concentration of standard working solution internal standard composition azithromycin-D3, unit are micro- gram per liter (μ g/L)；
ci-- the concentration of solution internal standard composition azithromycin-D3 in sample, unit are micro- gram per liter (μ g/L)；
As-- the peak area of azithromycin standard working solution；
The peak area of azithromycin in A-- sample；
Asi-- the peak area of azithromycin standard working solution internal standard composition azithromycin-D3；,
Ai-- the peak area of azithromycin-D3 in sample；
V-- sample constant volume, unit are milliliter (mL)；
M-- sample sample weighting amount, unit are gram (g).
Calculated result needs to deduct blank value, when being as a result less than 0.3 μ g/kg, is considered as and is not detected.
The detection method of azithromycin residual quantity in livestock and poultry hair described above, the method is in detection livestock and poultry hair
Using the livestock and poultry are preferably the fowl poultry kinds such as chicken, pig, ox, most preferably preferably chicken.
Technical solution of the present invention has the advantages that
1. the detection method of azithromycin residual quantity in animal hair provided by the invention is detection pair with animal hair
As realizing livestock and poultry In vivo detection without livestock and poultry such as slaughter chicken, pig, oxen；Hair sample is compared with muscle, liver, the acquisitions side such as excrement
Just, and since growth cycle of hair is long, more it can accurately monitor whether growth of animals or poultry process uses azithromycin, to realize livestock and poultry
Etc. food safety productions supervise purpose, testing result is accurate, situations such as being not in false positive, false negative, high sensitivity.
2. the detection method of azithromycin residual quantity in animal hair provided by the invention, by selecting special ratios formic acid
And methanol mixed solution, it enables to hair sample to be hydrolyzed at room temperature, shortens the drug pre-treatment time；In addition, addition
A certain amount of hydrogen peroxide can further shorten hydrolysis time, and hair sample hydrolysis extraction conditions are mild, easy, time saving.
3. the present invention modifies Fe using poly- divinylbenzene sulfonic acid-vinyl pyrrolidone (MCX)3O4Nano material magnetic suck
Azithromycin, absorption and purification efficiency are high, can be substantially reduced matrix effect, improve sensitivity, solve hair hydrolysis liquid hardly possible
In centrifugation and blocking solid phase extraction column problem.
4. the detection method of azithromycin residual quantity in livestock and poultry hair provided by the invention, which uses medical yarn
Cloth wraps up hair cleaning, filtering, has greatly saved the pre-treatment time, easy to operate.In addition, avoiding cleaning using hospital gauze
Trichomadesis in the process, sampling amount is minimum to can reach 0.1g, injures to livestock and poultry few.
5. the detection method of azithromycin residual quantity in animal hair provided by the invention, using " three-level gradient " journey
Sequence improves the detection sensitivity of this method by the selection of adjustment and sample hydrolysising condition etc. to elution program, detection
It is limited to 0.3 μ g/kg.
Detailed description of the invention
The poly- divinylbenzene sulfonic acid of Fig. 1-vinyl pyrrolidone (MCX) modifies Fe3O4The scanning electron microscope of nano material
Figure；
Fig. 2 positive chicken feather sample and the more reaction detections of internal standard compound (MRM) chromatogram；
Fig. 3 feminine gender chicken feather sample and the more reaction detections of internal standard compound (MRM) chromatogram；
Fig. 4 azithromycin standard items and the more reaction detections of internal standard compound (MRM) chromatogram.
Specific embodiment
There is provided following embodiments is to preferably further understand the present invention, it is not limited to the best embodiment party
Formula is not construed as limiting the contents of the present invention and protection scope, anyone under the inspiration of the present invention or by the present invention and its
The feature of his prior art is combined and any and identical or similar product of the present invention for obtaining, all falls within of the invention
Within protection scope.
Specific experiment step or condition person are not specified in embodiment, according to the literature in the art described routine experiment
The operation of step or condition can carry out.Reagents or instruments used without specified manufacturer, being can be by commercially available acquisition
Conventional reagent product.
Embodiment
The detection method of azithromycin residual quantity in animal hair provided by the invention, is realized especially by following steps:
1, poly- divinylbenzene sulfonic acid-vinyl pyrrolidone (MCX) modifies Fe3O4The preparation of nano material:
Take 2.70gFeCl3·6H2O and 1.39FeSO4·7H2O is dissolved in 200mL water by 2:1 (molar ratio), is passed through nitrogen
Gas shielded 20min~30min is added the poly- divinylbenzene sulfonic acid of 1.0g-vinyl pyrrolidone (MCX), is heated to 80 DEG C, rapidly
25.0mL ammonium hydroxide is added, continues to stir 30min, with secondary water and ethyl alcohol alternately cleaning 4 times, magnet separation, gained nano material
It is freeze-dried spare.
2, azithromycin equation of linear regression and detection limit
Configuration concentration is a series of azithromycin standard working solutions of 0.05 μ of μ g/L~100.0 g/L, internal standard Zitromax
Element-D3 concentration is 20.0 μ g/L, is mapped with peak area ratio (y) to content (x), the results showed that, in 0.05 μ of μ g/L~100.0 g/L
In range, peak area ratio (y) and azithromycin concentration are in good linear relationship.The linear equation of azithromycin is y=
0.02356x+0.01484, correlation coefficient r 2=0.9985.
Azithromycin standard solution is added in blank livestock and poultry hair sample, is detected by the method for foundation, according to
To azithromycin chromatographic peak signal-to-noise ratio calculate method minimum detection limit (s/n=3) be 0.3 μ g/kg, quantitative limit (s/n
It=10) is 1.0 μ g/kg.
3, the rate of recovery and precision
The blank livestock and poultry hair of azithromycin is not detected as sample substrate, in 1.0 μ g/kg, 5.0 μ g/kg, 20.0 μ
Tri- contents levels of g/kg add azithromycin standard specimen, and the rate of recovery, each pitch-based sphere are measured and calculated by aforementioned test methods
It is measured in parallel 6 times.Test measures the azithromycin rate of recovery in 95.6%~103.2% range, relative standard deviation 3.5%~
4.6%, as a result meet " GB27404-2008 Good Laboratory controls specification food Physico-chemical tests " about retention analysis requirement.Ah
The measuring method rate of recovery and relative standard deviation of miramycin are shown in Table 1.
The azithromycin measuring method rate of recovery and relative standard deviation (n=6) in 1 livestock and poultry hair of table
4, sample measures
The 8 parts of positive chicken feather samples, 4 parts that oral azithromycin dispersible tablet feeds are taken not to be fed for the chicken feather of azithromycin
Sample is detected according to following method.
The preparation of test solution: a. cleaning: chicken feather sample 0.5g is weighed, 0.1mg is accurate to, is placed in two layers of hospital gauze
In, with 15mL methanol, 15mL 0.1% (v/v) aqueous formic acid, 15mL secondary water is successively cleaned, is extracted；B. it hydrolyzes: taking cleaning
Good chicken feather sample shreds, and is placed in 50mL plastic centrifuge tube, be added 20.0 μ L1.0mg/L azithromycin-D3 working solutions and
(v/v) formic acid of 20.0mL 3.0% methanol solution (wherein containing hydrogen peroxide, volumetric concentration 0.3%), room temperature ultrasound
60min obtains chicken feather hydrolyzate；C. thickening-purification technology: chicken feather hydrolyzate is filtered with two layers of hospital gauze, blown in 50 DEG C of nitrogen it is close dry,
10.0mL0.1mol/LpH5.0 acetate buffer dissolved residue is added, the poly- divinylbenzene sulfonic acid-vinyl pyrrole of 25.0mg is added
Alkanone (MCX) modifies Fe3O4Nano material, after magnetic suck, Magneto separate discards acetate buffer.It is washed with 2.0mL5% ammoniated methanol
De- nano material, blows in 50 DEG C of nitrogen and closely does, and with 1.0mL methanol+water (1+1, v/v) dissolved residue, 0.22 μm of filter membrane is crossed, as confession
Test sample solution.
The detection of high performance liquid chromatography-tandem mass method:
Liquid phase chromatogram condition: chromatographic column: Agilent Eclipse plus C18,2.1mm × 100mm, 1.8 μm；Flowing
Phase A is containing 0.1% (v/v) aqueous formic acid, and Mobile phase B is methanol, flow velocity: 0.4mL/min；Column temperature: 35 DEG C；Sample volume:
10.0μL；Gradient elution program:: 0-2min, 2%B linear change to 40%B；2~3min keeps 40%B, 3~4min,
40%B linear change is to 75%B；4-5min keeps 75%B, 5~5.1min, 75%B linear change to 98%B；5.1-
6min keeps 98%B；6-6.1min98% is reduced to 2%B；6.1~7.0min maintains 2%B.
Mass Spectrometry Conditions: electric spray ion source, cation scan pattern；More reaction detections: spray voltage: 3000V, ion source
Temperature, 150 DEG C, sheath temperature degree: 300 DEG C；Sheath throughput: 12L/min.The quota ion of azithromycin be m/z749.5 >
591.4, qualitative ion is that the quota ion of m/z749.5 > 158 and azithromycin-D3 are m/z752.4 > 594.4.
It detects in above-mentioned sample containing azithromycin residual quantity between 6.5 μ of μ g/kg~258.6 g/kg, does not feed Archie
Azithromycin residual is not detected in the chicken feather sample of mycin, and part chromatogram is shown in Fig. 2-4, illustrates that the detection method has feasibility.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And thus amplify out it is obvious variation or
It changes still within the protection scope of the invention.
Claims (9)
1. the detection method of azithromycin residual quantity in a kind of animal hair, which comprises the following steps:
The preparation of test solution
Animal hair sample is taken, is cleaned, is shredded, mixed with azithromycin-D3 working solution, then addition formic acid mixes molten with methanol
Liquid, room temperature 30~60min of ultrasound obtain hair extracting solution, filter, drying, acetate buffer dissolved residue, poly- divinylbenzene sulphur
Acid-vinyl pyrrolidone modifies Fe3O4Nano material magnetic solid phase extraction, ammoniated methanol elution, drying are molten with methanol aqueous solution
Residue is solved, filtering obtains test solution；
The detection of high performance liquid chromatography-tandem mass method
High-efficient liquid phase chromatogram condition: chromatographic column: C18,2.1mm × 100mm, 1.8 μm；Mobile phase A is that volumetric concentration is 0.1% first
Aqueous acid, Mobile phase B are methanol, flow velocity: 0.4mL/min；Column temperature: 35 DEG C；Sample volume: 10 μ L；Gradient elution program: 0~
2min, 2%B linear change are to 40%B；2~3min keeps 40%B, 3~4min, 40%B linear change to 75%B；4-
5min keeps 75%B, 5~5.1min, 75%B linear change to 98%B；5.1-6min keeping 98%B；6-6.1min98%
It is reduced to 2%B；6.1~7.0min maintains 2%B；
Mass Spectrometry Conditions: electric spray ion source, cation scan pattern；More reaction detections: spray voltage: 3000V, ion source temperature
Degree, 150 DEG C, sheath temperature degree: 300 DEG C；Sheath throughput: 12L/min.
2. the detection method of azithromycin residual quantity in animal hair according to claim 1, which is characterized in that the first
For acid with methanol mixed solution, the volumetric concentration of formic acid is 2~4%.
3. the detection method of azithromycin residual quantity in animal hair according to claim 2, which is characterized in that the institute
It states in formic acid and methanol mixed solution and also contains hydrogen peroxide.
4. the detection method of azithromycin residual quantity in animal hair according to claim 3, which is characterized in that the mistake
The volume fraction of hydrogen oxide is 0.1%~0.5%.
5. the detection method of azithromycin residual quantity in animal hair according to claim 1, which is characterized in that the second
The pH of acid buffer is 4.0~5.0, and concentration is in 0.1~0.2mol/L, on the basis of the dosage of animal hair, acetate buffer
Dosage in 15-40mL/g.
6. the detection method of azithromycin residual quantity in animal hair according to claim 1, which is characterized in that described poly-
Divinylbenzene sulfonic acid-vinyl pyrrolidone modifies Fe3O4The preparation method of nano material is, by FeCl3And FeSO4By mole
It is dissolved in the water than 2:1, is passed through nitrogen protection 20min~30min, by every mM of poly- divinylbenzene sulphur of 0.05~0.2g of addition
Acid-vinyl pyrrolidone is heated to 80 DEG C, is rapidly added ammonium hydroxide, continues to stir 30min~60min, with secondary water and ethyl alcohol
It alternately cleans, magnet separation, the freeze-drying of gained nano material is spare.
7. the detection method of azithromycin residual quantity in animal hair according to claim 1, which is characterized in that the ammonia
Changing ammonium hydroxide in methanol, volume fraction is 2.0~5.0% in methyl alcohol.
8. the detection method of azithromycin residual quantity, feature exist in animal hair according to claim 1-7
In on the basis of the dosage of animal hair, the dosage of the methanol and formic acid mixed solution is 40~60mL/g, the Zitromax
The dosage of element-D3 working solution is 20~100 μ L/g, and the concentration of azithromycin-D3 working solution is 0.5~4.0mg/L.
9. the detection method of azithromycin residual quantity, feature exist in animal hair according to claim 1-8
In the quota ion of azithromycin is m/z749.5 > 591.4 in the Mass Spectrometry Conditions, and qualitative ion is the He of m/z749.5 > 158
The quota ion of azithromycin-D3 is m/z752.4 > 594.4.
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