CN109060993B - Method for detecting residual quantity of azithromycin in animal hair - Google Patents
Method for detecting residual quantity of azithromycin in animal hair Download PDFInfo
- Publication number
- CN109060993B CN109060993B CN201811022714.7A CN201811022714A CN109060993B CN 109060993 B CN109060993 B CN 109060993B CN 201811022714 A CN201811022714 A CN 201811022714A CN 109060993 B CN109060993 B CN 109060993B
- Authority
- CN
- China
- Prior art keywords
- azithromycin
- animal hair
- detecting
- solution
- methanol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
- G01N30/14—Preparation by elimination of some components
-
- 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
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
-
- 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
- G01N2030/042—Standards
- G01N2030/045—Standards internal
-
- 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
- G01N2030/062—Preparation extracting sample from raw material
-
- 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
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
Abstract
The invention belongs to the technical field of drug residue detection, and particularly relates to a method for detecting azithromycin residue in animal hair. The method takes animal hair as a detection object, does not need to slaughter chickens, pigs, cattle and other livestock and poultry, and realizes the live detection of the livestock and poultry; compared with muscles, livers, excrement and the like, the hair sample is convenient to obtain, and the growth cycle of the hair is long, so that whether the azithromycin is used in the growth process of the livestock and poultry can be accurately monitored, the purpose of monitoring the safe production of the food such as the livestock and poultry is achieved, the detection result is accurate, the situations of false positive, false negative and the like cannot occur, and the sensitivity is high.
Description
Technical Field
The invention belongs to the technical field of drug residue detection, and particularly relates to a method for detecting azithromycin residue in animal hair.
Background
Azithromycin (AZM) is a new generation macrolide antibiotic, acts by inhibiting protein synthesis, and is clinically used for preventing and treating human upper and lower respiratory tract, urinary tract, skin and soft tissue infection and sexually transmitted diseases. The compound has the characteristics of wide antibacterial spectrum, long half-life period, stability in an acidic environment and the like, the local veterinary drug standard in China has been recorded in 2004, and the compound is listed in a forbidden veterinary drug list by the Ministry of agriculture in 2005.
The azithromycin is illegally used for livestock and poultry breeding, which can affect the prevention and treatment of livestock and poultry epidemic diseases and the safety of livestock and poultry products, increase the risk of drug resistance generated by bacteria and threaten the health of human beings. Although the state is forbidden, the economic benefit is damaged due to the breeding environment, so that farmers still add antibiotics into the feed or use the antibiotics through other ways, and the antibiotics for human use are still abused on livestock and poultry, which becomes a new hidden danger threatening the safety of livestock and poultry products.
Researchers at home and abroad have carried out partial research on the detection technology of azithromycin in a matrix, but no detection standard about azithromycin in any matrix is issued yet. The detection methods which are researched more include an ultraviolet detection method, a fluorescence detection method and an isotope internal standard method, but the method of adopting an ultraviolet detector has weak absorption and extremely low sensitivity; the method using a fluorescence detector requires derivatization and takes time for measurement; and the method is rapid, simple and convenient, has strong specificity and high sensitivity by adopting an isotope internal standard method and high performance liquid chromatography-tandem mass spectrometry detection, and is a detection method which is more advocated in the current research.
At present, substrates for detecting azithromycin in livestock and poultry products are mainly muscle, liver, blood and excrement, the muscle and the liver need to be obtained by slaughtering live animals, livestock and poultry blood samples need to be obtained by professionals, and cold chain storage is needed before detection to prevent deterioration; the excrement is easy to be polluted and the sampling is inconvenient. Furthermore, drug residues in these matrices are difficult to detect after the drug holiday. The hair has the advantages that due to the structural component characteristics and the lower metabolic activity of the hair, the medicine is slowly metabolized after entering the hair, the medicine can be accumulated and retained for a long time, the long residual time is realized in the hair of livestock and poultry, the hair is convenient to sample and transport, and compared with muscle, liver, blood and excrement matrixes, the hair matrix is more suitable to be used as a detection sample to provide a more reliable confirmation basis for the supervision of forbidden medicines in the safety production of poultry products. At present, no method for detecting the residual quantity of azithromycin in the hair of livestock and poultry is available.
Disclosure of Invention
Therefore, the invention aims to overcome the defects that the detection result of the azithromycin in the livestock and poultry products in the prior art is unreliable, is not beneficial to the safety supervision of the livestock and poultry products, and the detection sample is not easy to obtain or store, and the like, thereby providing the method for detecting the azithromycin residue in the animal hair.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for detecting azithromycin residual quantity in animal hair comprises the following steps:
1. preparation of test solution
Putting a hair sample into a double-layer medical gauze, cleaning, cutting into pieces, mixing with azithromycin-D3 working solution, adding a mixed solution of formic acid and methanol, carrying out ultrasonic treatment at room temperature for 30-60 min to obtain a hair extracting solution, filtering, drying, dissolving residues with an acetic acid buffer solution, and modifying Fe with polydivinylbenzene sulfonic acid-vinyl pyrrolidone (MCX)3O4Performing magnetic solid phase extraction on the nano material, eluting with ammoniated methanol, drying, dissolving the residue with 1mL of methanol aqueous solution (1:1, v/v), and filtering with a filter membrane to obtain a test solution;
2. high performance liquid chromatography-tandem mass spectrometry detection
High performance liquid chromatography conditions: a chromatographic column: c18, 2.1mm × 100mm,1.8 μm; the mobile phase A is 0.1% formic acid aqueous solution by volume concentration, the mobile phase B is methanol, and the flow rate is as follows: 0.4 mL/min; column temperature: 35 ℃; sample introduction amount: 10 mu L of the solution; gradient elution procedure: linearly changing the 2% B to 40% B in 0-2 min; keeping for 2-3 min, keeping for 40% B, and keeping for 3-4 min, wherein 40% B is linearly changed to 75% B; keeping 75% B for 4-5min, and linearly changing 75% B to 98% B for 5-5.1 min; keeping 98% B for 5.1-6 min; 98% is reduced to 2% B at 6-6.1 min; maintaining 2% of B for 6.1-7.0 min;
mass spectrum conditions: electrospray ion source, positive ion scan mode; and (3) multi-reaction detection: spraying voltage: 3000V, ion source temperature, 150 ℃, sheath gas temperature: 300 ℃; the flow rate of the sheath gas: 12L/min.
Preferably, the volume concentration of the formic acid in the methanol mixed solution of the formic acid and the methanol is 2-4%.
Preferably, the mixed solution of methanol and formic acid further contains hydrogen peroxide, and the volume fraction of the hydrogen peroxide is 0.1-0.5%.
Preferably, the pH of the acetic acid buffer solution is 4.0-5.0, the concentration is 0.1-0.2 mol/L, and the dosage of the acetic acid buffer solution is 15-40mL/g based on the dosage of the animal hair.
Preferably, the polydivinylbenzenesulfonic acid-vinylpyrrolidone (MCX) modifies Fe3O4The dosage of the nano material is 20.0-100.0 mg, and the preparation method comprises the following step of mixing FeCl3And FeSO4Dissolving the nano material into water according to a molar ratio of 2:1 (mol ratio), introducing nitrogen for protection for 20min to 30min, adding 0.05 to 0.2g of polydivinylbenzenesulfonic acid-vinyl pyrrolidone (MCX) into each millimole, heating to 80 ℃, rapidly adding ammonia water, continuously stirring for 30min to 60min, alternately cleaning with secondary water and ethanol, separating by using a magnet, and freeze-drying the obtained nano material for later use.
Preferably, the ammonia water in the ammoniated methanol has a volume fraction of 2.0-5.0% in the methanol, and the dosage is 2.0-5.0 mL.
Preferably, the dosage of the mixed solution of the methanol and the formic acid is 40-60 mL/g based on the dosage of the animal hair, the dosage of the azithromycin-D3 working solution is 20-100 mu L/g, and the concentration of the azithromycin-D3 working solution is 0.5-4.0 mg/L.
Preferably, the quantitative ions of the azithromycin in the mass spectrum conditions are m/z749.5>591.4, the qualitative ions of the azithromycin are m/z749.5>158, and the quantitative ions of the azithromycin-D3 are m/z752.4> 594.4.
The invention calculates the residual quantity of azithromycin in hair by peak area according to an internal standard method, and the calculation formula is as follows:
x- -residual amount of azithromycin in the sample in micrograms per kilogram (μ g/kg);
c- -concentration of azithromycin standard working fluid in units of micrograms per liter (μ g/L);
csi-concentration of azithromycin-D3 as an internal standard for standard working solutions in micrograms per liter (μ g/L);
ci-concentration of azithromycin-D3 as an internal standard of solution in micrograms per liter (μ g/L) in the sample;
As-peak area of azithromycin standard working solution;
a-the peak area of azithromycin in the sample;
Asi-peak area of azithromycin-D3 as an internal standard of azithromycin standard working solution; a
Ai-peak area of azithromycin-D3 in the sample;
v- -sample volume fixed volume in milliliters (mL);
m- -sample weight in grams (g).
If the calculation result requires subtraction of blank value and the result is less than 0.3. mu.g/kg, it is considered as undetected.
The method for detecting the azithromycin residue in the livestock hair is applied to the detection of the livestock hair, and the livestock is preferably livestock such as chicken, pig, cattle and the like, and is most preferably chicken.
The technical scheme of the invention has the following advantages:
1. the method for detecting the azithromycin residual quantity in the animal hair provided by the invention takes the animal hair as a detection object, does not need to slaughter chickens, pigs, cattle and other livestock and poultry, and realizes the live detection of the livestock and poultry; compared with muscles, livers, excrement and the like, the hair sample is convenient to obtain, and the growth cycle of the hair is long, so that whether the azithromycin is used in the growth process of the livestock and poultry can be accurately monitored, the purpose of monitoring the safe production of the food such as the livestock and poultry is achieved, the detection result is accurate, the situations of false positive, false negative and the like cannot occur, and the sensitivity is high.
2. According to the method for detecting the azithromycin residue in the animal hair, the mixed solution of formic acid and methanol in a specific ratio is selected, so that the hair sample can be hydrolyzed at room temperature, and the pretreatment time of the medicine is shortened; in addition, the addition of a certain amount of hydrogen peroxide can further shorten the hydrolysis time, and the hair sample hydrolysis extraction condition is mild, simple and convenient, and time-saving.
3. The invention adopts polydivinylbenzene sulfonic acid-vinyl pyrrolidone (MCX) to modify Fe3O4The nano material magnetic adsorption azithromycin has high adsorption and purification efficiency, can obviously reduce matrix effect, improve sensitivity and solve the problems that the hair hydrolysate is difficult to centrifuge and block a solid phase extraction column.
4. According to the method for detecting the azithromycin residue in the livestock and poultry hair, the hair is wrapped by medical gauze, cleaned and filtered, so that the pretreatment time is greatly saved, and the operation is simple and convenient. In addition, the medical gauze avoids hair loss in the cleaning process, the minimum sampling amount can reach 0.1g, and the damage to livestock and poultry is less.
5. The method for detecting the azithromycin residue in the animal hair adopts a three-level elution gradient program, improves the detection sensitivity of the method by adjusting the elution program, selecting the hydrolysis conditions of the sample and the like, and has the detection limit of 0.3 mug/kg.
Drawings
FIG. 1 polydivinylbenzenesulfonic acid-vinylpyrrolidone (MCX) modified Fe3O4Scanning electron microscopy of the nanomaterial;
FIG. 2 is a multi-reaction detection (MRM) chromatogram of a positive chicken feather sample and an internal standard;
FIG. 3 Multi-reaction detection (MRM) chromatogram of a negative chicken feather sample and an internal standard;
figure 4 Azithromycin standard and internal standard multi-reaction detection (MRM) chromatogram.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Examples
The invention provides a method for detecting azithromycin residual quantity in animal hair, which is realized by the following steps:
1. fe modified by polydivinylbenzenesulfonic acid-vinylpyrrolidone (MCX)3O4Preparing a nano material:
taking 2.70g FeCl3·6H2O and 1.39FeSO4·7H2Dissolving O in 200mL of water according to a molar ratio of 2:1, introducing nitrogen for protection for 20 min-30 min, adding 1.0g of polydivinylbenzenesulfonic acid-vinyl pyrrolidone (MCX), heating to 80 ℃, rapidly adding 25.0mL of ammonia water, continuously stirring for 30min, alternately cleaning for 4 times by using secondary water and ethanol, separating by using a magnet, and freeze-drying the obtained nano material for later use.
2. Azithromycin linear regression equation and detection limit
A series of azithromycin standard working solutions with the concentration of 0.05 mu g/L-100.0 mu g/L are prepared, the concentration of the internal standard azithromycin-D3 is 20.0 mu g/L, and the peak area ratio (y) is plotted against the content (x), so that the result shows that the peak area ratio (y) and the azithromycin concentration have good linear relation in the range of 0.05 mu g/L-100.0 mu g/L. The linear equation of the azithromycin is that y is 0.02356x +0.01484, and the correlation coefficient r2 is 0.9985.
Adding an azithromycin standard solution into a blank livestock and poultry hair sample, detecting according to an established method, and calculating the lowest detection limit (s/n is 3) of the method to be 0.3 mu g/kg and the quantitative limit (s/n is 10) to be 1.0 mu g/kg according to the obtained signal-to-noise ratio of the azithromycin chromatographic peak.
3. Recovery and precision
Taking blank livestock and poultry hair without azithromycin detection as a sample matrix, adding azithromycin standard samples at three content levels of 1.0 mug/kg, 5.0 mug/kg and 20.0 mug/kg, measuring and calculating the recovery rate according to the test method, and parallelly measuring each addition level for 6 times. The test shows that the azithromycin recovery rate is in the range of 95.6-103.2 percent, the relative standard deviation is 3.5-4.6 percent, and the result meets the requirements of GB27404-2008 laboratory quality control standard food physicochemical detection on residue analysis. The determination method of azithromycin has the recovery rate and relative standard deviation shown in the table 1.
TABLE 1 determination of azithromycin in animal hair recovery rate and relative standard deviation (n ═ 6)
4. Sample assay
8 parts of positive chicken feather samples obtained by feeding the oral azithromycin dispersible tablets and 4 parts of chicken feather samples which are not fed with azithromycin are detected according to the following method.
Preparation of a test solution: a. cleaning: weighing 0.5g of chicken feather sample, accurately measuring the weight of the chicken feather sample to 0.1mg, placing the chicken feather sample in a double-layer medical gauze, sequentially cleaning the chicken feather sample by using 15mL of methanol, 15mL of 0.1% (v/v) formic acid aqueous solution and 15mL of secondary water, and squeezing the chicken feather sample; b. hydrolysis: cutting cleaned chicken feather samples into pieces, placing the cut chicken feather samples into a 50mL plastic centrifuge tube, adding 20.0 mu L of 1.0mg/L azithromycin-D3 working solution and 20.0mL of 3.0% (v/v) methanoic acid solution (containing hydrogen peroxide and having the volume concentration of 0.3%), and performing ultrasonic treatment at room temperature for 60min to obtain chicken feather hydrolysate; c. concentration and purification: filtering the chicken feather hydrolysate with two layers of medical gauze, blowing to dry at 50 deg.C under nitrogen, adding 10.0 ml/L0.1 mol/L pH5.0 acetic acid buffer solution to dissolve residue, adding 25.0mg polydivinylbenzenesulfonic acid-vinyl pyrrolidone (MCX) to modify Fe3O4And magnetically adsorbing the nano material, and magnetically separating to remove the acetic acid buffer solution. The nanomaterial was eluted with 2.0mL of 5% ammoniated methanol, nitrogen-blown to dryness at 50 ℃ and the residue was dissolved with 1.0mL of methanol + water (1+1, v/v), and the resulting solution was filtered through a 0.22 μm filter to prepare a test solution.
Detecting by using a high performance liquid chromatography-tandem mass spectrometry method:
liquid chromatography conditions: a chromatographic column: agilent Eclipse plus C18, 2.1mm × 100mm,1.8 μm; the mobile phase A is aqueous solution containing 0.1% (v/v) formic acid, the mobile phase B is methanol, and the flow rate: 0.4 mL/min; column temperature: 35 ℃; sample introduction amount: 10.0 μ L; gradient elution procedure: : 0-2min, 2% B linear change to 40% B; keeping for 2-3 min, keeping for 40% B, and keeping for 3-4 min, wherein 40% B is linearly changed to 75% B; keeping 75% B for 4-5min, and linearly changing 75% B to 98% B for 5-5.1 min; keeping 98% B for 5.1-6 min; 98% is reduced to 2% B at 6-6.1 min; maintaining 2% B for 6.1-7.0 min.
Mass spectrum conditions: electrospray ion source, positive ion scan mode; and (3) multi-reaction detection: spraying voltage: 3000V, ion source temperature, 150 ℃, sheath gas temperature: 300 ℃; the flow rate of the sheath gas: 12L/min. The quantitative ion of the azithromycin is m/z749.5>591.4, the qualitative ion of the azithromycin is m/z749.5>158 and the quantitative ion of the azithromycin-D3 is m/z752.4> 594.4.
The residual quantity of the azithromycin contained in the sample is detected to be between 6.5 and 258.6 mu g/kg, the residual azithromycin is not detected in the chicken feather sample which is not fed with the azithromycin, and partial chromatograms are shown in figures 2 to 4, thereby showing that the detection method has feasibility.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.
Claims (8)
1. A method for detecting the residual quantity of azithromycin in animal hair is characterized by comprising the following steps:
preparation of test solution
Taking an animal hair sample, cleaning, cutting into pieces, mixing with azithromycin-D3 working solution, adding a mixed solution of formic acid, hydrogen peroxide and methanol, carrying out ultrasonic treatment at room temperature for 30-60 min to obtain a hair extracting solution, filtering, drying, dissolving in an acetic acid buffer solutionDecomposing residues, and modifying Fe by polydivinyl benzene sulfonic acid-vinyl pyrrolidone3O4Performing magnetic solid phase extraction on the nano material, eluting by ammoniated methanol, drying, dissolving residues by using a methanol water solution, and filtering to obtain a test solution;
high performance liquid chromatography-tandem mass spectrometry detection
High performance liquid chromatography conditions: a chromatographic column: c18, 2.1mm × 100mm,1.8 μm; the mobile phase A is 0.1% formic acid aqueous solution by volume concentration, the mobile phase B is methanol, and the flow rate is as follows: 0.4 mL/min; column temperature: 35 ℃; sample introduction amount: 10 mu L of the solution; gradient elution procedure: linearly changing the 2% B to 40% B in 0-2 min; keeping for 2-3 min, keeping for 40% B, and keeping for 3-4 min, wherein 40% B is linearly changed to 75% B; keeping 75% B for 4-5min, and linearly changing 75% B to 98% B for 5-5.1 min; keeping 98% B for 5.1-6 min; 98% is reduced to 2% B at 6-6.1 min; maintaining 2% of B for 6.1-7.0 min;
mass spectrum conditions: electrospray ion source, positive ion scan mode; and (3) multi-reaction detection: spraying voltage: 3000V, ion source temperature, 150 ℃, sheath gas temperature: 300 ℃; the flow rate of the sheath gas: 12L/min.
2. The method for detecting the residual quantity of azithromycin in animal hair according to claim 1, characterized in that the volume concentration of formic acid in the mixed solution of formic acid, hydrogen peroxide and methanol is 2-4%.
3. The method for detecting the residual amount of azithromycin in animal hair, as claimed in claim 2, wherein the volume fraction of hydrogen peroxide is 0.1-0.5%.
4. The method for detecting the residual quantity of the azithromycin in the animal hair as claimed in claim 1, wherein the pH of the acetic acid buffer solution is 4.0-5.0, the concentration is 0.1-0.2 mol/L, and the dosage of the acetic acid buffer solution is 15-40mL/g based on the dosage of the animal hair.
5. The method for detecting the residual amount of azithromycin in animal hair according to claim 1, wherein the method comprises the step of detecting the residual amount of azithromycin in animal hairFe modified by polydivinylbenzenesulfonic acid-vinyl pyrrolidone3O4The preparation method of the nano material comprises the steps of adding FeCl3And FeSO4Dissolving the nano material in water according to the molar ratio of 2:1, introducing nitrogen for protection for 20min to 30min, adding 0.05 to 0.2g of polydivinylbenzenesulfonic acid-vinyl pyrrolidone into each millimole, heating to 80 ℃, rapidly adding ammonia water, continuously stirring for 30min to 60min, alternately cleaning with secondary water and ethanol, separating by using a magnet, and freeze-drying the obtained nano material for later use.
6. The method for detecting the residual amount of azithromycin in animal hair according to claim 1, wherein the ammonia water in the ammoniated methanol has a volume fraction of 2.0-5.0% in methanol.
7. The method for detecting the residual quantity of the azithromycin in the animal hair as claimed in any one of claims 1 to 6, wherein the dosage of the mixed solution of the methanol, the hydrogen peroxide and the formic acid is 40 to 60mL/g, the dosage of the azithromycin-D3 working solution is 20 to 100 μ L/g, and the concentration of the azithromycin-D3 working solution is 0.5 to 4.0mg/L based on the dosage of the animal hair.
8. The method for detecting the residual quantity of azithromycin in animal hair as claimed in claim 7, wherein the quantitative ions of azithromycin in the mass spectrum condition are m/z749.5>591.4, the qualitative ions are m/z749.5>158 and the quantitative ions of azithromycin-D3 are m/z752.4> 594.4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811022714.7A CN109060993B (en) | 2018-09-03 | 2018-09-03 | Method for detecting residual quantity of azithromycin in animal hair |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811022714.7A CN109060993B (en) | 2018-09-03 | 2018-09-03 | Method for detecting residual quantity of azithromycin in animal hair |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109060993A CN109060993A (en) | 2018-12-21 |
| CN109060993B true CN109060993B (en) | 2021-06-25 |
Family
ID=64759538
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811022714.7A Active CN109060993B (en) | 2018-09-03 | 2018-09-03 | Method for detecting residual quantity of azithromycin in animal hair |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109060993B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103675145A (en) * | 2013-12-18 | 2014-03-26 | 广西壮族自治区分析测试研究中心 | Method for detecting residual quantity of cimaterol in pig hairs |
| CN104155398A (en) * | 2014-08-21 | 2014-11-19 | 江西省农业科学院农产品质量安全与标准研究所 | Method for detecting residual quantity of antivirus drug in hairs of livestock and poultry |
| CN108283918A (en) * | 2018-02-13 | 2018-07-17 | 上海市刑事科学技术研究院 | Magnetic microsphere and its scared detection application |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2014276460A1 (en) * | 2013-06-04 | 2015-12-24 | Vyome Biosciences Pvt. Ltd. | Coated particles and compositions comprising same |
-
2018
- 2018-09-03 CN CN201811022714.7A patent/CN109060993B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103675145A (en) * | 2013-12-18 | 2014-03-26 | 广西壮族自治区分析测试研究中心 | Method for detecting residual quantity of cimaterol in pig hairs |
| CN104155398A (en) * | 2014-08-21 | 2014-11-19 | 江西省农业科学院农产品质量安全与标准研究所 | Method for detecting residual quantity of antivirus drug in hairs of livestock and poultry |
| CN108283918A (en) * | 2018-02-13 | 2018-07-17 | 上海市刑事科学技术研究院 | Magnetic microsphere and its scared detection application |
Non-Patent Citations (4)
| Title |
|---|
| Depletion Study of Enrofloxacin and Its Metabolite Ciprofloxacin in Edible Tissues and Feathers of White Leghorn Hens by Liquid Chromatography Coupled with Tandem Mass Spectrometry;B. SAN MARTIN等;《Journal of Food Protection》;20071231;第70卷(第8期);第1952-1957页 * |
| Drug Screening of Hair by Liquid Chromatography-Tandem Mass Spectrometry;S. Hegstad等;《Journal of Analytical Toxicology》;20080630;第32卷;第364-372页 * |
| Further Assessment of PPCPs in Feed Grade Chicken Feather Meal Including Potential Sources;Zhixin Chen;《A Thesis Presented to the Graduate School of Clemson University》;20151231;第15-20,71页 * |
| 液相色谱-串联质谱法测定育肥猪配合饲料中的阿奇霉素;唐祥等;《分析测试学报》;20170331;第36卷(第3期);第363页第1.4节和表1 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109060993A (en) | 2018-12-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Høverstad et al. | Short-chain fatty acids in germfree mice and rats | |
| CN101846661B (en) | Method for simultaneously measuring residual quantities of lincomycin and macrolides in royal jelly | |
| Schramm et al. | Synthesis of cellulose by Acetobacter xylinum. 1. Micromethod for the determination of celluloses | |
| CN104155398B (en) | A kind of method detecting antiviral drugs residual quantity in livestock and poultry hair | |
| Nabuurs et al. | A long-term perfusion test to measure net absorption in the small intestine of weaned pigs | |
| CN114563507B (en) | Treatment method, detection method and application of beta-receptor agonist residues in animal tissues | |
| Smith et al. | Analysis of volatile emissions from porcine faeces and urine using selected ion flow tube mass spectrometry | |
| CN109709258B (en) | Method for detecting florfenicol total residues in edible tissues of pigs and application | |
| CN109060993B (en) | Method for detecting residual quantity of azithromycin in animal hair | |
| Zhanteng et al. | Residue accumulation, distribution, and withdrawal period of sulfamethazine and N-acetylsulfamethazine in poultry waste from broilers | |
| Sohlberg et al. | Plasma concentrations of flumequine after intra-arterial and oral administration to rainbow trout (Salmo gairdneri) exposed to low water temperatures | |
| CN109060994B (en) | Method for detecting residual amount of ofloxacin in livestock and poultry hair | |
| CN103675145B (en) | Method for detecting residual quantity of cimaterol in pig hairs | |
| Kabir et al. | Estimation of apparent digestibility coefficients in rainbow trout (Oncorhynchus mykiss) using different markers: 1. Validation of microtracer F–Ni as a marker | |
| CN110658279A (en) | Method for detecting ribavirin and metabolites thereof in livestock and poultry hair | |
| CN109142576A (en) | The detection method of roxithromycin residual quantity in a kind of animal hair | |
| Sadeh et al. | Induced mannosidosis‐excretion of oligosaccharides by locoweed‐intoxicated sheep | |
| CN107389843B (en) | Method for detecting dihydropyridine in feed | |
| CN103130875B (en) | Method for extracting polymyxin B from fermentation broth | |
| CN112526024A (en) | Method for detecting sulfonamide antibiotics and acetylated metabolites thereof in aquatic products | |
| CN104792899B (en) | Method for detecting residue of multiple quinolones in feed by adopting HPLC-ESI-MS/MS process | |
| Martinez et al. | Determination of monensin sodium residues in beef liver tissue by liquid chromatography of a fluorescent derivative | |
| Deverall et al. | Metabolism of Indoleacetic Acid in Rust Diseases. II. Metabolites of Carboxyl-labeled Indoleacetic Acid in Tissues | |
| CN109580818B (en) | Method for detecting florfenicol drug residue in pig hair | |
| CN109932460A (en) | The remaining detection method of tylosin in a kind of tissue |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |