CN109298109A - In meat product a variety of beasts it is residual and meanwhile detection method - Google Patents
In meat product a variety of beasts it is residual and meanwhile detection method Download PDFInfo
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- CN109298109A CN109298109A CN201811491960.7A CN201811491960A CN109298109A CN 109298109 A CN109298109 A CN 109298109A CN 201811491960 A CN201811491960 A CN 201811491960A CN 109298109 A CN109298109 A CN 109298109A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The present invention relates to the residual detection technique field of beast, provide that a variety of beasts in a kind of meat product are residual while the method for detection, including sample treatment；Establish standard curve；The content that each beast is residual in institute's sample is calculated according to standard curve；Detection method is HPLC-MS method.Whereby, the present invention is by using PLS-A solid phase extraction column, without activation and equilibrium step, extracting solution, which is directly over pillar just, can remove the matrix interference object of removing protein, salt, phosphatide etc. 95% or more, most of veterinary drugs can all extract to realize different types of beast residual by a pre-treatment directly by being not preserved.Pre-treatment step is simplified, without activating to solid-phase extraction column, and multiclass residue of veterinary drug can be detected simultaneously, substantially reduce the pre-treatment time, reduce testing cost.The result shows that this method is accurate, quick, easy, quantitative result is reliable, it is very suitable to handle multiple batches of sample simultaneously.
Description
Technical field
Residual the present invention relates to a variety of beasts in the residual detection technique field of beast more particularly to a kind of meat product while detection side
Method.
Background technique
Mainly there are sulfamido, quinolones, Tetracyclines, beta receptor in China using more veterinary drug in terms of livestock-raising
The compounds such as agonist class, chloromycetin, malachite green class, pentachloro- phenolic acid sodium.It abuses these drugs and easily causes livestock products
Serious pollution, and entered in the animal derived foods such as muscle by metabolic pathway, it is accumulated in human body eventually by food chain, and
And these drugs have and lead to allergic reaction and make the side effects such as human body develops drug resistance.Therefore, a variety of veterinary drugs are monitored in meat system
Residual in product has positive effect to guarantee food safety.
Currently, detection method is divided into according to veterinary drug type mostly while relevant criterion and more residues of veterinary drug reported in the literature
Several detection method, the veterinary drug of multiple types, which tests and analyzes to be limited by simultaneously, to be lacked unified pre-treating method and can not achieve,
And most methods pretreatment process is cumbersome, the rate of recovery is low, and can not detect a variety of residues of veterinary drug simultaneously.
In summary, the existing technology has inconveniences and defects in actual use, so it is necessary to be improved.
Summary of the invention
For above-mentioned defect, residual the purpose of the present invention is to provide a variety of beasts in a kind of meat product while detection side
Method is directly over pillar and just can remove by using PLS-A solid phase extraction column without activation and equilibrium step, extracting solution
The matrix interference object of albumen, salt, phosphatide etc. 95% or more, most of veterinary drugs can be directly by being not preserved, to realize not
Congener beast residual all extracts by a pre-treatment.Pre-treatment step is simplified, without living to solid-phase extraction column
Change, and multiclass residue of veterinary drug can be detected simultaneously, substantially reduces the pre-treatment time, reduce testing cost.The result shows that the party
Method is accurate, quick, easy, quantitative result is reliable, is very suitable to handle multiple batches of sample simultaneously.
To achieve the goals above, the present invention provides that a variety of beasts in a kind of meat product are residual while the method for detection, including
Sample treatment: taking 2.50g sample, and 10mL extracting solution is added, and vibrates 5min, and ultrasonic 5min, 5000rpm are centrifuged 5min, in taking-up
Clear liquid is added in SPE pillar or QuEChERS is purified in pipe, then receives efflux；By received efflux in 50 DEG C of water bath conditions
Lower nitrogen is blown to 0.5mL or so, is settled to 1mL with constant volume liquid, crosses 0.22 μm of miillpore filter；The SPE pillar is PLS-A column；
Take machine testing on the liquid filtered out；
Establish standard curve: the preparation of preparation and matrix matching standard curve including hybrid standard working solution；
It is 100 μ g/ that the preparation of hybrid standard working solution:, which weighing a variety of veterinary drug standard items of equivalent, and is configured to concentration respectively
Single mark standard solution of mL；Every kind of single mark standard solution takes 50 μ L, and is settled to 5ml, and obtaining concentration is 1.0 μ g/mL mixing mark
Quasi- product working solution；500 μ L concentration are taken to be 1.0ug/mL hybrid standard product working solution and be settled to 5mL, obtaining concentration is 0.1 μ g/mL
Hybrid standard product working solution；
The preparation of matrix matching mixed standard solution: precision measure 0.1 μ g/mL hybrid standard working solution, 20 μ L and 50 μ L with
And 10 μ L of 1.0ug/mL hybrid standard working solution, 20 μ L, 50 μ L and 100 μ L, it is then respectively adding in a blank sample, obtains 6
Part mark-on sample；6 parts of mark-on samples are dried with nitrogen through 50 DEG C of water-baths respectively, solution of reordering respectively later dissolution residue is simultaneously diluted to
1mL obtains the matrix matching mixing that concentration is respectively 1ng/mL, 5ng/mL, 10ng/mL, 20ng/mL, 50ng/mL and 100ng/mL
Standard solution；
Each matrix matching mixed standard solution is gone up into machine testing respectively, is ordinate by the characteristic ion peak area measured,
Corresponding concentration of standard solution is abscissa, draws standard curve；
The content that each beast is residual in institute's sample is calculated according to standard curve；
The upper machine testing method is HPLC-MS method.
In meat product according to the present invention a variety of beasts it is residual and meanwhile detection method, the upper machine testing includes: cation
Mode and negative ion mode；
Positive ion mode:
Chromatographic condition
Chromatographic column: C18 chromatographic column (1.9 μm, 100 × 2.1mm)；Mobile phase: A: acetonitrile, C: the water of 0.1% formic acid of addition
Solution；Flow velocity: 0.25mL/min；Column temperature: 40 DEG C；Sample volume: 5 μ L；Gradient elution；
Mass Spectrometry Conditions:
Negative ion mode:
Chromatographic condition:
Chromatographic column: C18 chromatographic column (1.9 μm, 100 × 2.1mm)；Mobile phase: A: acetonitrile, C: water；Flow velocity: 0.25mL/
min；Column temperature: 40 DEG C；Sample volume: 5 μ L；Gradient elution；
Mass Spectrometry Conditions:
In meat product according to the present invention a variety of beasts it is residual and meanwhile detection method, a variety of veterinary drugs be sulfamido, quinoline
Promise ketone, Tetracyclines, beta receptor agonist class, chloromycetin, malachite green class and pentachloro- phenolic acid sodium class.
In meat product according to the present invention a variety of beasts it is residual and meanwhile detection method, a variety of veterinary drugs be 32 kinds, respectively
It is husky for Terbutaline, salbutamol, sulphadiazine, sulfamethyldiazine, trimethoprim, Norfloxacin, Ofloxacin, training fluorine
Star, tetracycline, Ciprofloxacin, terramycin, Ractopamine, Lomefloxacin, Enrofloxacin, sulfadimidine, sarafloxacin,
Aureomycin, Clenbuterol, daimeton, cistosulfa, fanasil, sulfamethoxazole, strength are mould
Element, Tilmicosin, madribon, sulfaquinoxaline, leucogentian violet, malachite green, Thiamphenicol, fluorobenzene Buddhist nun
It examines, chloramphenicol and pentachloro- phenolic acid sodium.
A variety of beasts are residual in meat product according to the present invention while the method for detection, and the SRM condition of 32 kinds of veterinary drugs is shown in
Table 2.
In meat product according to the present invention a variety of beasts it is residual and meanwhile detection method, the constant volume liquid be acetonitrile.
A variety of beasts are residual in meat product according to the present invention while the method for detection, the extracting solution preferably contain 0.1%
90% acetonitrile water of formic acid.
A variety of beasts are residual in meat product according to the present invention while the method for detection, and the condition of gradient elution is shown in Table 1.
In meat product according to the present invention a variety of beasts it is residual and meanwhile detection method, the meat be the flesh of fish.
Residual the purpose of the present invention is to provide a variety of beasts in a kind of meat product while detection method, by using PLS-
A solid phase extraction column, without activation and equilibrium step, extracting solution, which is directly over pillar just, can remove removing protein, salt, phosphatide etc.
95% or more matrix interference object, most of veterinary drugs can be directly by being not preserved, to realize different types of beast residual
It is all extracted by a pre-treatment.Pre-treatment step is simplified, without being activated to solid-phase extraction column, and can be detected simultaneously
Multiclass residue of veterinary drug substantially reduces the pre-treatment time, reduces testing cost.The result shows that this method is accurate, quick, letter
Just, quantitative result is reliable, is very suitable to handle multiple batches of sample simultaneously.
Detailed description of the invention
Fig. 1 is the typical chromatogram of Terbutaline of the invention；
Fig. 2 is the typical chromatogram of salbutamol of the invention；
Fig. 3 is the typical chromatogram of sulphadiazine of the invention；
Fig. 4 is the typical chromatogram of sulfamethyldiazine of the invention；
Fig. 5 is the typical chromatogram of trimethoprim of the invention；
Fig. 6 is the typical chromatogram of Norfloxacin of the invention；
Fig. 7 is the typical chromatogram of Ofloxacin of the invention；
Fig. 8 is the typical chromatogram of pefloxacin of the invention；
Fig. 9 is the typical chromatogram of tetracycline of the invention；
Figure 10 is the typical chromatogram of Ciprofloxacin of the invention；
Figure 11 is the typical chromatogram of terramycin of the invention；
Figure 12 is the typical chromatogram of Ractopamine of the invention；
Figure 13 is the typical chromatogram of Lomefloxacin of the invention；
Figure 14 is the typical chromatogram of Enrofloxacin of the invention；
Figure 15 is the typical chromatogram of sulfadimidine of the invention；
Figure 16 is the typical chromatogram of sarafloxacin of the invention；
Figure 17 is the typical chromatogram of aureomycin of the invention；
Figure 18 is the typical chromatogram of Clenbuterol of the invention；
Figure 19 is the typical chromatogram of daimeton of the invention；
Figure 20 is the typical chromatogram of cistosulfa of the invention；
Figure 21 is the typical chromatogram of fanasil of the invention；
Figure 22 is the typical chromatogram of sulfamethoxazole of the invention；
Figure 23 is the typical chromatogram of fortimicin of the invention；
Figure 24 is the typical chromatogram of Tilmicosin of the invention；
Figure 25 is the typical chromatogram of madribon of the invention；
Figure 26 is the typical chromatogram of sulfaquinoxaline of the invention；
Figure 27 is the typical chromatogram of leucogentian violet of the invention；
Figure 28 is the typical chromatogram of malachite green of the invention；
Figure 29 is the typical chromatogram of Thiamphenicol of the invention；
Figure 30 is the typical chromatogram of Florfenicol of the invention；
Figure 31 is the typical chromatogram of chloramphenicol of the invention；
Figure 32 is the typical chromatogram of pentachloro- phenolic acid sodium of the invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The present invention provides that a variety of beasts in a kind of meat product are residual while the method for detection, includes the following steps:
Sample treatment: taking 2.50g sample, and 10mL extracting solution is added, and vibrates 5min, ultrasonic 5min, 5000rpm centrifugation
5min takes out in supernatant addition SPE pillar or in QuEChERS purification pipe, then receives efflux；Received efflux is existed
Nitrogen is blown to 0.5mL or so under 50 DEG C of water bath conditions, is settled to 1mL with constant volume liquid, crosses 0.22 μm of miillpore filter；
Take machine testing on the liquid filtered out；
Establish standard curve: the preparation of preparation and matrix matching standard curve including hybrid standard working solution；
It is 100 μ g/ that the preparation of hybrid standard working solution:, which weighing a variety of veterinary drug standard items of equivalent, and is configured to concentration respectively
Single mark standard solution of mL；Every kind of single mark standard solution takes 50 μ L, and is settled to 5ml, and obtaining concentration is 1.0 μ g/mL mixing mark
Quasi- product working solution；It takes 500 μ L1.0ug/mL hybrid standard product working solutions and is settled to 5mL, obtaining concentration is 0.1 μ g/mL mixing mark
Quasi- product working solution；
The present invention uses acetonitrile constant volume.
The preparation of matrix matching mixed standard solution: precision measures 0.1 μ g/mL hybrid standard working solution, 20 μ L and 50 μ L,
10 μ L of 1.0ug/mL hybrid standard working solution, 20 μ L, 50 μ L and 100 μ L, are then respectively adding in a blank sample, obtain 6 parts
Mark-on sample；6 parts of mark-on samples are dried with nitrogen through 50 DEG C of water-baths respectively, solution of reordering respectively later dissolution residue is simultaneously diluted to
1mL obtains the matrix matching mixing that concentration is respectively 1ng/mL, 5ng/mL, 10ng/mL, 20ng/mL, 50ng/mL and 100ng/mL
Standard solution；
Each matrix matching mixed standard solution is gone up into machine testing respectively, is ordinate by the characteristic ion peak area measured,
Corresponding concentration of standard solution is abscissa, draws standard curve；
The content that each beast is residual in institute's sample is calculated according to standard curve；
Upper machine testing method of the invention is HPLC-MS method.
Embodiment, the present invention carry out the foundation of the standard curve of a variety of veterinary drugs using preceding method selection flesh of fish sample.Choosing
It is sulfamido, quinolones, Tetracyclines, beta receptor agonist class, chloromycetin, malachite green class and pentachloro- phenolic acid with veterinary drug
Sodium class.32 kinds of specific choice, respectively Terbutaline, salbutamol, sulphadiazine, sulfamethyldiazine, trimethoprim, promise fluorine
Sha Xing, Ofloxacin, pefloxacin, tetracycline, Ciprofloxacin, terramycin, Ractopamine, Lomefloxacin, Enrofloxacin, sulphur
Amine diformazan pyrimidine, sarafloxacin, aureomycin, Clenbuterol, daimeton, cistosulfa, sulfanilamide (SN) neighbour's dimethoxy are phonetic
Pyridine, sulfamethoxazole, fortimicin, Tilmicosin, madribon, sulfaquinoxaline, leucogentian violet, peacock
Malachite green, Thiamphenicol, Florfenicol, chloramphenicol and pentachloro- phenolic acid sodium.
The instrument and equipment that the present invention uses includes: (the U.S. liquid chromatography mass combined instrument TSQ Quantum Ultra
Thermo Fisher Scientific company)；C18 chromatographic column (100 × 2.1mm, 1.9 μm of particle size, Thermo
Fisher Scientific company)；GTCS-2013B vertical oscialltor (ring high-tech automatic technology research institute of Beijing state)；KQ-
700DE type numerical control ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.)；TGL-20M refrigerated centrifuge (Hunan Kai Dake
Learn Instrument Ltd.)；EA32 type multifunctional sample concentrating instrument (Beijing Polytech Instrument Co., Ltd.).
The reagent that the present invention uses includes: acetonitrile (chromatographically pure), formic acid (chromatographically pure), Watson ultrapure water；Extracting solution:
90% acetonitrile water (contains 0.1% formic acid)；Determine solution: 10% acetonitrile water.
Present invention acetonitrile, ethyl acetate, 90% acetonitrile water or 90% acetonitrile water (containing 0.1% formic acid), solution extracted sample
Product, discovery can be residual while having certain protein precipitation with all beasts are effectively extracted with 90% acetonitrile water (containing 0.1% formic acid)
Effect.Therefore, extracting solution of the invention is preferably the 90% acetonitrile water for containing 0.1% formic acid.
The SPE pillar that the present invention selects is PLS-A column.PLS-A column has extremely strong water logging lubricant nature, is a kind of water logging lubricant nature suction
Attached dose, analyte can directly interact with it, can also obtain when directly aqueous sample is loaded on adsorbent
Retain.It can eliminate the need for activation and equilibrium step required when silica matrix or other polymer absorbants.Save these volumes
After outer step, the adsorbent without water logging lubricant nature can not be effectively retained target analytes in loading step, so as to cause
The low rate of recovery.Valuable sample processing time can be saved by saving these steps, and can be saved solvent and be reduced liquid waste processing expense
With.
According to conventional methods such as national standards, which needs to be extracted with different method respectively, then with different
Purification column purification.Quinolones, Tetracyclines, chloromycetin need to use HLB Solid Phase Extraction column purification, and sulfamido, beta receptor swash
Dynamic agent class needs to be purified with MCX mixed type cation exchange column, malachite green class is needed with neutral alumina column purification, pentachlorophenol
Sour sodium is needed with MAX mixed type anion exchange column purification.
The experiment that seven pre-treatments are needed according to national standard can be reduced to using PAS-A column can by a pre-treatment
Complete, detection efficiency mention it is seven times higher, experiment consumables cost reduce by seven times.
Upper machine testing includes: positive ion mode and negative ion mode；
Positive ion mode:
Chromatographic condition
Chromatographic column: C18 chromatographic column (1.9 μm, 100 × 2.1mm)；Mobile phase: A: acetonitrile, C: the water of 0.1% formic acid of addition
Solution；Flow velocity: 0.25mL/min；Column temperature: 40 DEG C；Sample volume: 5 μ L；Gradient elution；
Mass Spectrometry Conditions:
Negative ion mode:
Chromatographic condition:
Chromatographic column: C18 chromatographic column (1.9 μm, 100 × 2.1mm)；Mobile phase: A: acetonitrile, C: water；Flow velocity: 0.25mL/
min；Column temperature: 40 DEG C；Sample volume: 5 μ L；Gradient elution；
Condition of gradient elution of the invention is shown in Table 1.
1 gradient elution of table
Inventor has investigated the separating effect of each component when column temperature is 25 DEG C, 30 DEG C, 35 DEG C and 40 DEG C, and discovery column temperature is herein
Can be efficiently separated in range, as temperature increases, appearance time slightly shortens, but column temperature be 40 DEG C when each component peak shape point
Sharp and separating degree is preferable, therefore selects column temperature for 40 DEG C.
Mass Spectrometry Conditions:
The SRM condition of 32 kinds of veterinary drugs includes: that qualitative ion pair, quota ion pair, collision gas energy and Tubelens are utilized
TSQ Tune software optimizes the SRM condition of 32 kinds of veterinary drugs respectively, finds optimal parameter, is shown in Table 2.
2 SRM condition of table
The typical chromatogram of 32 kinds of veterinary drug standard specimens is shown in Fig. 1-Figure 32.
The range of linearity and detection limit of standard curve
Aforementioned mixed standard solution is analyzed.The concentration of each mixed standard solution is respectively 1ng/mL, 5ng/mL, 10ng/
ML, 20ng/mL, 50ng/mL and 100ng/mL, it is final to obtain six groups of test results.Using solution concentration as abscissa, with corresponding peak
Area is that ordinate carries out linear regression.Regression equation, related coefficient, detection limit and the range of linearity are shown in Table 3.
As shown in Table 3, related coefficient generally meets or exceeds 0.9985；Detection limit: 1.0-3.0 μ g/kg；Linearly
Range 1-20mg/L.
The rate of recovery, precision: as shown in Table 4, the rate of recovery of 32 kinds of veterinary drugs of the invention is that 85.3~104.7%, RSD is
2.4~8.9%.
Result above is it is found that detection method of the invention meets the requirement of national standard.
In HPLC-MS detection, there are large effect, stronger matrix effects for accuracy of the matrix effect to testing result
Reply result can produce biggish deviation.Matrix effect is matrix mark and solvent target ratio, and the present invention is found through experiments that, promise
Flucloxacillin, single promise sand star, Enrofloxacin, tetracycline, there are ion humidification, other 27 kinds of chemical combination for 5 kinds of compounds of terramycin
There is ion inhibiting effect in object.But matrix effect generally acts on smaller, illustrates that the clean-up effect of pre-treatment is good, to targeted
Closing object and inhibiting or enhance ionization matrix has preferable separating degree.
Detection method of the invention is unlimited to be also applied for the meats such as pork, beef, chicken or duck with the flesh of fish.
3 directrix curve regression equation of table, related coefficient and detection limit
4 rate of recovery of table and precision
In conclusion residual the purpose of the present invention is to provide a variety of beasts in a kind of meat product while detection method, leads to
Cross using PLS-A solid phase extraction column, without activation and equilibrium step, extracting solution be directly over pillar just and can go removing protein,
The matrix interference object of salt, phosphatide etc. 95% or more, most of veterinary drugs can be directly by being not preserved, to realize variety classes
Beast residual all extract by a pre-treatment.Pre-treatment step is simplified, without being activated to solid-phase extraction column, and energy
Multiclass residue of veterinary drug is detected simultaneously, the pre-treatment time is substantially reduced, reduces testing cost.The result shows that this method it is accurate,
Quickly, simplicity, quantitative result are reliable, are very suitable to handle multiple batches of sample simultaneously.
Certainly, the present invention can also have other various embodiments, without deviating from the spirit and substance of the present invention, ripe
It knows those skilled in the art and makes various corresponding changes and modifications, but these corresponding changes and change in accordance with the present invention
Shape all should fall within the scope of protection of the appended claims of the present invention.
Claims (9)
1. in a kind of meat product a variety of beasts it is residual and meanwhile detection method, which comprises the steps of:
Sample treatment: taking 2.50g sample, and 10mL extracting solution is added, and vibrates 5min, and ultrasonic 5min, 5000rpm are centrifuged 5min, take
Supernatant is added in SPE pillar out or QuEChERS is purified in pipe, then receives efflux；By received efflux in 50 DEG C of water-baths
Under the conditions of nitrogen be blown to 0.5mL or so, be settled to 1mL with constant volume liquid, cross 0.22 μm of miillpore filter；The SPE pillar is PLS-A
Column；
Take machine testing on the liquid filtered out；
Establish standard curve: the preparation of preparation and matrix matching standard curve including hybrid standard working solution；
It is 100 μ g/mL's that the preparation of hybrid standard working solution:, which weighing a variety of veterinary drug standard items of equivalent, and is configured to concentration respectively
Single mark standard solution；Every kind of single mark standard solution takes 50 μ L, and is settled to 5ml, and obtaining concentration is 1.0 μ g/mL hybrid standard product
Working solution；It takes 500 μ L concentration to be 1.0ug/mL hybrid standard product working solution and be settled to 5mL, obtains concentration as 0.1 μ g/mL mixing
Standard items working solution；
The preparation of matrix matching mixed standard solution: precision measure 0.1 μ g/mL hybrid standard working solution, 20 μ L and 50 μ L and
10 μ L of 1.0ug/mL hybrid standard working solution, 20 μ L, 50 μ L and 100 μ L, are then respectively adding in a blank sample, obtain 6 parts
Mark-on sample；6 parts of mark-on samples are dried with nitrogen through 50 DEG C of water-baths respectively, solution of reordering respectively later dissolution residue is simultaneously diluted to
1mL obtains the matrix matching mixing that concentration is respectively 1ng/mL, 5ng/mL, 10ng/mL, 20ng/mL, 50ng/mL and 100ng/mL
Standard solution；
Each matrix matching mixed standard solution is gone up into machine testing respectively, is ordinate by the characteristic ion peak area measured, it is corresponding
Concentration of standard solution be abscissa, draw standard curve；
The content that each beast is residual in institute's sample is calculated according to standard curve；
The upper machine testing method is HPLC-MS method.
2. in meat product according to claim 1 a variety of beasts it is residual and meanwhile detection method, which is characterized in that the upper machine
Detection includes: positive ion mode and negative ion mode；
Positive ion mode:
Chromatographic condition
Chromatographic column: C18 chromatographic column；Mobile phase: A: acetonitrile, C: the aqueous solution of 0.1% formic acid of addition；Flow velocity: 0.25mL/min；Column
Temperature: 40 DEG C；Sample volume: 5 μ L；Gradient elution；
Mass Spectrometry Conditions:
Negative ion mode:
Chromatographic condition:
Chromatographic column: C18 chromatographic column；Mobile phase: A: acetonitrile, C: water；Flow velocity: 0.25mL/min；Column temperature: 40 DEG C；Sample volume: 5 μ L；
Gradient elution；
Mass Spectrometry Conditions:
3. in meat product according to claim 2 a variety of beasts it is residual and meanwhile detection method, which is characterized in that it is described a variety of
Veterinary drug is sulfamido, quinolones, Tetracyclines, beta receptor agonist class, chloromycetin, malachite green class and pentachloro- phenolic acid sodium
Class.
4. in meat product according to claim 3 a variety of beasts it is residual and meanwhile detection method, which is characterized in that it is described a variety of
Veterinary drug is 32 kinds, respectively Terbutaline, salbutamol, sulphadiazine, sulfamethyldiazine, trimethoprim, Norfloxacin, oxygen
Flucloxacillin, pefloxacin, tetracycline, Ciprofloxacin, terramycin, Ractopamine, Lomefloxacin, Enrofloxacin, sulfanilamide (SN) diformazan
Pyrimidine, sarafloxacin, aureomycin, Clenbuterol, daimeton, cistosulfa, fanasil, sulfanilamide (SN)
First oxazole, fortimicin, Tilmicosin, madribon, sulfaquinoxaline, leucogentian violet, malachite green, first
Hyrazin, Florfenicol, chloramphenicol and pentachloro- phenolic acid sodium.
5. in meat product according to claim 4 a variety of beasts it is residual and meanwhile detection method, which is characterized in that described 32 kinds
The SRM condition of veterinary drug see the table below.
6. in meat product according to claim 1 a variety of beasts it is residual and meanwhile detection method, which is characterized in that the constant volume
Liquid is acetonitrile.
7. in meat product according to claim 1 a variety of beasts it is residual and meanwhile detection method, which is characterized in that the extraction
Liquid is preferably the 90% acetonitrile water for containing 0.1% formic acid.
8. in meat product according to claim 2 a variety of beasts it is residual and meanwhile detection method, which is characterized in that the gradient
Elution requirement see the table below.
9. a variety of beasts are residual in meat product described in any one according to claim 1~8 while the method for detection, feature exists
In the meat is the flesh of fish, pork, beef, chicken or duck.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109738559A (en) * | 2019-03-06 | 2019-05-10 | 烟台大学 | Methanol saltout split-phase extract meat products in quinolones residual pre-treating method |
| CN109991337A (en) * | 2019-04-30 | 2019-07-09 | 湖北出入境检验检疫局检验检疫技术中心 | The method for detecting four class drugs and its metabolin in Eriocheir sinensis crab cream simultaneously |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109738559A (en) * | 2019-03-06 | 2019-05-10 | 烟台大学 | Methanol saltout split-phase extract meat products in quinolones residual pre-treating method |
| CN109991337A (en) * | 2019-04-30 | 2019-07-09 | 湖北出入境检验检疫局检验检疫技术中心 | The method for detecting four class drugs and its metabolin in Eriocheir sinensis crab cream simultaneously |
| CN109991337B (en) * | 2019-04-30 | 2022-03-18 | 武汉海关技术中心 | Method for simultaneously detecting four drugs and metabolites thereof in crab cream of Eriocheir sinensis |
| CN112684067A (en) * | 2020-12-10 | 2021-04-20 | 山东大学 | Method for simultaneously detecting multiple antibiotic residues in aquatic product |
| CN112924588A (en) * | 2021-01-27 | 2021-06-08 | 浙江公正检验中心有限公司 | Detection method for simultaneous determination of chloramphenicols and pentachlorophenol in livestock and poultry products |
| CN114200053A (en) * | 2021-12-10 | 2022-03-18 | 碳元复兴(厦门)科技有限公司 | Method for simultaneously detecting residues of various veterinary drugs in biogas slurry |
| CN115128180A (en) * | 2022-05-31 | 2022-09-30 | 江苏康达检测技术股份有限公司 | Unified detection method for determining multiple PPCPs in water sample |
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