CN109358130A - A kind of remaining method of azithromycin in measurement poultry livers tissue - Google Patents
A kind of remaining method of azithromycin in measurement poultry livers tissue Download PDFInfo
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- CN109358130A CN109358130A CN201811503169.3A CN201811503169A CN109358130A CN 109358130 A CN109358130 A CN 109358130A CN 201811503169 A CN201811503169 A CN 201811503169A CN 109358130 A CN109358130 A CN 109358130A
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- G—PHYSICS
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- 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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Abstract
The invention discloses a kind of remaining methods of azithromycin in measurement poultry livers tissue, belong to medicament residue detection technique field.It is to be remained using after the azithromycin in acetonitrile, n-hexane, NaCl extraction sample to be tested using HPLC-MS/MS detection azithromycin that the present invention, which measures the remaining method of azithromycin in poultry livers tissue,.The present invention is directed to the characteristic of poultry livers, probes into the process flow for sample and simplification, the reagent consumptive material simplification for reducing the operation difficulty of experiment, using improve treatment effeciency；On the other hand optimization Liquid Chromatography-Tandem Mass Spectrometry parameter, realizes the qualitative and quantitative analysis of 0.1 μ g/kg trace in sample.
Description
Technical field
The invention belongs to medicament residue detection technique fields, and in particular to azithromycin in a kind of measurement poultry livers tissue
Remaining method.
Background technique
Azithromycin (azithromycin) belongs to second generation macrolide antibiotics, is existed by Pliva company of Yugoslavia
The end of the eighties in last century researches and develops successfully.Azithromycin is since its tolerance is preferable, and adverse reaction rate is lower, application clinically
Widely.
Azithromycin is erythromycin chemical structure by modification as a kind of semi-synthetic fifteen-membered ring lactone antibiotic
A kind of broad-spectrum antibiotic obtained later is mainly used for all kinds of inflammation or infectious diseases caused by bacterium.
Azithromycin in conjunction with the 50S large subunit of bacterial ribosome by inhibiting bacterio protein to synthesize, from spatially
Retardance new polypeptide chain extends and pt-tRNA is promoted to fall off, and acyltransferase polypeptide tRNA is inhibited to be displaced from A to P, inhibits displacement enzyme, interference
Protein synthesis reaches antibacterial purpose.
With the rise of aquaculture industry of China, this drug using more and more common, its growth, anti-in food-borne animal
Cancer, antibiosis play an important role, and have long-range application prospect.This drug comparatively Small side effects, main needle
The organs such as liver are had an impact.
Liver has the efficiency such as synthesis, removing toxic substances, immune, storage, and liver has different degrees of after poultry medication
Medicament residue, azithromycin cure the newest antibacterials that clinic control uses as people and are used for food animal, can generate drug resistance
Problem influences animal epidemic control, food safety and human health.Since animal tissue's especially liver organization comparison of ingredients is multiple
Miscellaneous, sample impurity not only influences analyte detection to be measured, but also may damage the service life of instrument reduction detection device, does thus
Good its, which detects work, seems increasingly important.
Up to the present, the rare report of correlative study in relation to azithromycin in carcass liver method for detecting residue, the country
There are no the unified standard of azithromycin maximum residue limit in animal food and efficiently and effectively detection method.The country to Ah
Miramycin is quantified mainly for preparation (tablet, injection etc.) pharmaceutically, and that has inquired into many detection azithromycins has efficacious prescriptions
Method.
Existing the Sanitation Ministry medicine standard and provincial standard is for identification one used by macrolide antibiotics
As be ultraviolet spectrophotometry, but this method lacks specificity to the analysis of antibiotic, it is easy to cause to examine mistake and
It is chaotic.
Macrolide antibiotic residues measurement side in present standard SN/T 1777.2-2007 animal derived food
Enrofloxacin, Danofloxacin, Ciprofloxacin, sarafloxacin, Orbifloxacin, two in method, GB/T22985-2008 milk and milk powder
Although the measurement of Flucloxacillin and marbofloxacin residual quantity has used Liquid Chromatography-Tandem Mass Spectrometry technology, further improve analysis
Specificity, but lack azithromycin in analysis project and lack the residual research to poultry liver.
Xu Guangwei etc. reports the remaining method of azithromycin in a kind of efficient liquid phase-ultraviolet method detection Broiler Tissues；
Blue red plum et al. was registered HPLC-MS method measurement azithromycin in human plasma and its pharmacokinetics；Grain is strong-willed et al. to register
QuEChERS- high performance liquid chromatography-tandem mass method measures the remaining method of azithromycin in animal-derived food；The above related inspection
Survey method, it is accurately, reproducible, but detection detection limit is relatively high and special place is carried out to poultry livers tissue without specific aim
Reason analysis and research.
Patent CN 107228912A discloses a kind of screening method of 79 kinds of antibacterials in animal food, specifically adopts
Medicament residue is detected with liquid chromatography mass after organic solvent extraction, Solid Phase Extraction, the LOD of this method azithromycin is 0.5 μ
G/kg, LOQ are 2 μ g/kg；Macrolide antibiotics tylosin, Tilmicosin, Ji in the chicken liver tissue of this method detection
He is limited to 10 μ g/kg at quantifying for mycin A5；Although this method is related to the azithromycin residue detection of poultry livers, detection limit
It is high.
Data is shown at present, external remaining to azithromycin in the animal bodies such as cat, horse, sheep, rabbit, chum salmon, boa
Quantitative detecting method expands research, and the quantification range of azithromycin is made to have reached 0.01 μ g/g.The ratio that foreign pharmacopeia records is turbid
Method, because turbidimetry is quicker than agar diffusion method, no spreading factor influences, Instrument measuring precision and high sensitivity, with chromatography string
Connection mass spectrometry quantitative technique more still has gap.Content reverse phase alumina column, ampere electricity of the U.S. to internal azithromycin
The detection of the methods of chemistry, it is minimum to be quantitatively limited to 1ng/g, but testing conditions are generally difficult to realize at home.
Currently, need it is a kind of for poultry livers matrix feature, provide it is quick, sensitive, reliable, accurate, be suitable for birds liver
The method of dirty azithromycin residue detection.
Summary of the invention
Aiming at the problems existing in the prior art, the purpose of the present invention is to provide a kind of quick, sensitive, reliable, accurate
Measurement poultry livers tissue in azithromycin method, provide quantitative square in the intracorporal pharmacokinetic of birds for drug
Method.
A kind of remaining method of azithromycin in measurement poultry livers tissue, steps are as follows:
(1) sample pre-treatments
The poultry livers tissue 2.00g (± 0.01) to be measured of homogenate is accurately weighed in 50mL centrifuge tube, the 5mL eddies of water is added
Rotation mix, be added 25mL acetonitrile, concussion extract 15min, then plus 5gNaCl, 10mL n-hexane, shake 5min, 4000r/min from
Heart 5min takes acetonitrile layer into 100mL pear shape bottle, 40 DEG C of rotary evaporated to dryness；
1mL methanol-water (1:1) constant volume is added in pear shape bottle, be vortexed ultrasound, takes constant volume liquid into 2mL centrifuge tube, is added 750
μ L acetonitrile is saturated n-hexane, is vortexed, and 0.45 μm of organic phase, water phase filter membrane are crossed by high speed centrifugation Hou Qu lower layer, to HPLC-MS/MS points
Analysis；
(2) HPLC-MS/MS is analyzed
Chromatographic condition:
Chromatographic column: Agilent EclipsePlus C18 (1.8 μm of 2.1*150mm)；Column temperature: 40 DEG C；
Mobile phase: flow path AB: methanol, the aqueous formic acid of flow path BA:0.1%；
Flow velocity: 0.3mL/min, sample volume: 2 μ L；
Gradient elution is as follows:
| Time | Flow path AB component (%) | Flow path BA component (%) |
| 0.10 | 20 | 80 |
| 1.00 | 20 | 80 |
| 3.00 | 80 | 20 |
| 3.50 | 80 | 20 |
| 3.51 | 20 | 80 |
| 4.00 | Stop |
Mass Spectrometry Conditions:
Type ion source: ESI (+)；
Nebulizing Gas Flow:3L/min；
Heating Gas:10L/min；
Interface Temperature:300 DEG C；
DL Temperature:250 DEG C；
Heat Block Temperature:400 DEG C；
Drving Gas Flow:10L/min.
Beneficial effects of the present invention
The present invention probes into simultaneously simplification in the process flow for sample, makes to reduce for the characteristic in poultry livers
The operation difficulty of experiment, the reagent consumptive material used are simplified, and treatment effeciency is improved；On the other hand optimization Liquid Chromatography-Tandem Mass Spectrometry
Parameter realizes the qualitative and quantitative analysis of 0.1 μ g/kg trace in sample.The addition of azithromycin is returned in actual experiment analysis
The rate of recovery of receipts is greater than 80%, and the coefficient of variation is respectively less than 5% and meets normal food detection demand in a few days and in the daytime.
Different animal tissue's matrix components are multifarious, have different influences for different pharmaceutical residue detection, lead to
It often will affect the rate of recovery or direct interference detection process of drug；A kind of method for detecting residue pair of animal tissue under normal conditions
In another kind tissue, there is also method applicability problems.The complexity of matrix be easy to cause the false positive or vacation for testing and analyzing result
It is negative；The complexity of matrix is the difficult point of poultry livers drug residue trace detection.Poultry livers tissue is compared with other position groups
Matrix complexity is knitted, a large amount of pigment, protein and fat etc. are contained in poultry livers and interferes matrix, and interferes the ingredient of matrix
It is more, content difference is big；These interference matrix components wide varieties, include inorganic matter, organic matter, ionic, highly polar compound
With non-polar compound etc.；In addition, poultry livers also contain multiple biological activities enzyme, pretreatment mode is improper will cause mesh for test
The decomposition of mark object, which is destroyed or combined by other substances, causes the low detection accuracy decline of the analysis test objective object rate of recovery or pollution to examine
The response of measurement equipment jamming target object.
Azithromycin belongs to alkaline compound, is soluble in acidic aqueous solution and polar organic solvent, in neutral aqueous solution
In it is relatively stable.5mL water vortex mixed is added during the extraction process, makes sample in liquid environment by test by the present invention
Fully dispersed increase is known as Zitromax preferably with the contact and distribution coefficient, the neutral liquid environment of test for extracting reagent
Stability ensures the higher rate of recovery and stability in detection；Azithromycin has biggish distribution coefficient in acetonitrile, using second
On the one hand nitrile obtains higher extraction efficiency as Extraction solvent, other hand keeps part albuminous degeneration in sample heavy by acetonitrile
It forms sediment, reaches clean-up effect.By the way that sodium chloride is added in test, realizes the distribution of liquid liquid, be soluble in n-hexane using oil substances
And n-hexane and the unmixing feature of acetonitrile, n-hexane is added in extraction process, removes the lipid impurities in sample.Reduce to point
The pollution of desorption device.
The method of the present invention distributes the principle of extraction based on liquid liquid, and appropriate adjustment extracts essence step in test, has ensured change
The stabilization for closing object has higher extraction efficiency；Test process does not need complex instrument equipment, swift to operate, easy, experimental cost
It is low.
The method of the present invention the rate of recovery and is had good stability by the experiments of different substrates；It can be used as animal-derived food birds
The method foundation that azithromycin medicament residue detects in liver can also be studied as reference in the medicine generation to azithromycin.
Detailed description of the invention
Fig. 1 difference proportion of mobile phase and azithromycin corresponding relation；
The mass spectrogram of Fig. 2 azithromycin；
The standard curve of Fig. 3 azithromycin.
Specific embodiment
Term as used in the present invention generally has those of ordinary skill in the art usual unless otherwise specified
The meaning of understanding.
Combined with specific embodiments below, and referring to the data further detailed description present invention.Following embodiment only be
It illustrates the present invention, rather than limits the scope of the invention in any way.
Embodiment
1. the configuration of standard solution
The preparation of 1.1 stock solutions
It accurately weighs azithromycin standard items 10mg to be placed in 10mL volumetric flask, dissolves constant volume with methanol, obtain containing Archie
The stock solution of mycin 1000mg/mL, -18 DEG C save backup.
The preparation of 1.2 standard intermediate fluids
1000mg/mL stock solution 1mL accurately is pipetted into 10mL volumetric flask, obtains 100mg/mL's with methanol dissolution constant volume
Intermediate fluid, -18 DEG C save backup.
The preparation of 1.3 working solutions
100mg/mL intermediate fluid 1mL accurately is pipetted into 10mL volumetric flask, obtains the work of 10mg/mL with methanol dissolution constant volume
Make liquid, -18 DEG C save backup.
The working solution for taking 10mg/mL, use initial flow Phase Proportion solvent (methanol: 0.1% aqueous formic acid 2: 8) as
Retarder thinner is configured to 0.1,0.5,1.0,5.0,10.0 μ g/mL standard solution of standard curve, to be analyzed.
2. animal specimen is handled
New freshly-slaughtered poultry, duck, Goose Liver several pieces, by (- 20 DEG C) storages of individual freezing.Group is used after shearing-crushing frustillatum
It knits refiner and carries out homogenate preparation, similar blank sample is carried out after analysis detection to test matrix as experiment after mixing,
It saves spare at extremely -20 DEG C.
The poultry livers tissue 2.00g (± 0.01) of homogenate is accurately weighed in 50mL centrifuge tube, it is mixed that the rotation of the 5mL eddies of water is added
It is even, be added 25mL acetonitrile, concussion extract 15min, then plus 5g NaCl, 10mL n-hexane, shake 5min, 4000r/min centrifugation
5min.Take acetonitrile layer into 100mL pear shape bottle, 40 DEG C of rotary evaporated to dryness.
1mL methanol-water (1:1) constant volume is added in pear shape bottle, be vortexed ultrasound, takes constant volume liquid into 2mL centrifuge tube, is added 750
μ L acetonitrile is saturated n-hexane, is vortexed, and 0.45 μm of organic phase, water phase filter membrane are crossed by high speed centrifugation Hou Qu lower layer, to HPLC-MS/MS points
Analysis.
3.HPLC-MS/MS analysis
Chromatographic condition:
Chromatographic column: Agilent EclipsePlus C18 (1.8 μm of 2.1*150mm)；Column temperature: 40 DEG C；
Mobile phase: flow path AB: methanol；The aqueous formic acid of flow path BA:0.1%；
Flow velocity: 0.3mL/min, sample volume: 2 μ L；
Gradient elution is as follows:
1 gradient elution of table
| Time | Flow path AB component (%) | Flow path BA component (%) |
| 0.10 | 20 | 80 |
| 1.00 | 20 | 80 |
| 3.00 | 80 | 20 |
| 3.50 | 80 | 20 |
| 3.51 | 20 | 80 |
| 4.00 | Stop |
Increase organic Phase Proportion by adjusting initial flow Phase Proportion and in the process, gradient elution initially uses 80% water
1min is mutually kept, so that the water-soluble polar impurity in sample is quickly flowed out control object and delays elution outflow, increase after 1min
Organic Phase Proportion reaches highest when organic Phase Proportion arrival 3min；This section of gradient by object appearance time control 2.5min extremely
Between 3min, chromatography peak stretching is controlled within 20s；To reach higher separating degree and lesser peak stretching, symmetric figure is obtained
Normal distribution curve peak type.
Mass Spectrometry Conditions:
Type ion source: ESI (+)；
Nebulizing Gas Flow:3L/min；
Heating Gas:10L/min；
Interface Temperature:300 DEG C；
DL Temperature:250 DEG C；
Heat Block Temperature:400 DEG C；
Drving Gas Flow:10L/min.
4. result and analysis
4.1 different proportion of mobile phase and azithromycin corresponding relation
Different water phases (pure water, 0.1% formic acid water) is selected, organic phase (methanol, acetonitrile) carries out standard substance analysis, often
Kind 6 statistics different ratios of mobile phase combinatory analysis and compound response relation are as shown in Figure 1.
As shown in Figure 1, water phase uses 0.1% aqueous formic acid, organic phase to use methanol, to the response of azithromycin
Highest.
4.2 specificity
The mass-spectrogram of azithromycin by mass spectrum as shown in Fig. 2, optimize to obtain 3 ion pairs, wherein ordinate is to ring
It answers, abscissa m/z.
By in electron spray cation and being born respectively using the azithromycin standard solution of 1mg/L to mass spectrum parameter optimization
Parent ion full scan is carried out under ion mode respectively, the results are shown in Table 2:
2 azithromycin MRM ion parameters of table
As shown in Table 2, the cation (ESI of azithromycin+[M+H]+M/Z:749.5) response is significantly larger than anion (ESI-
[M-H]-M/Z:748.0).It selects to carry out second order ms full scan to azithromycin under positive ion mode；Wherein, with 749.50 >
591.55 749.50 > of quota ion, 116.10,749.50 > 158.15 the most are qualitative ion.
4.3 standard substance is linear and response confirmation
0.1,0.5,1.0,5.0,10.0 μ g/mL of configuration standard curve analyzes result as shown in figure 3, in 0.1~10.0 μ g/
In L concentration range, linear relationship is good, R2 > 0.999.
5. adding recovery experiment
Stand-by homogenate sample in selection 2, carries out three horizontal (0.1,0.5,2.0 μ g/kg) addition recycling, and each level adds
Add sample size N=10, the rate of recovery is calculated, the results are shown in Table 3.
The rate of recovery=(theory addition concentration/analysis measures concentration) * 100%.
3 rate of recovery of table and stability confirmation
Three kinds of different birds internal organ are selected, three horizontal addition recycling are done to it, as a result know: azithromycin is in three kinds of bases
The rate of recovery in the horizontal addition recovery experiment of the three of matter is all larger than 80%, and lot-to-lot variability is less than 5%；Meet general analysis reality
Test detection demand.In the addition recovery experiment of 0.1 μ g/kg level, three kinds of different matrix object rate of recovery are in 80%-
Between 120%, and internal standard compound response S/N is much larger than 10, therefore 0.1 μ g/kg of setting method detection limit.
6. stability experiment
Replication is carried out according to 5 addition recovery experiments, selects different substrates in a few days repeat n=12 times, weighs in the daytime
N=6 times multiple, 5 standard curves are quantitative, calculate the rate of recovery and count rate of recovery RSD value, the results are shown in Table 4.
The azithromycin in a few days and in the daytime coefficient of variation in 4 poultry livers of table
As shown in Table 4, azithromycin residual quantity in a few days makes a variation dilute in three horizontal addition recovery experiments of three kinds of matrix
It releases and is distributed between 2.18~4.22%, the coefficient of variation is distributed between 3.25~4.86% in the daytime, in a few days and in the daytime variation lines
Number is respectively less than 5%, and the stability of method meets analysis requirement of experiment.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than is limited；Although referring to aforementioned reality
Applying example, invention is explained in detail, for those of ordinary skill in the art, still can be to aforementioned implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these are modified or replace
It changes, the spirit and scope for claimed technical solution of the invention that it does not separate the essence of the corresponding technical solution.
Claims (3)
1. a kind of remaining method of azithromycin in measurement poultry livers tissue, it is characterised in that: using acetonitrile, n-hexane,
After NaCl extracts the azithromycin in sample to be tested, using HPLC-MS/MS detection azithromycin residual；
The extracting method of azithromycin in the sample to be tested are as follows:
The poultry livers tissue 2.00g (± 0.01) to be measured of homogenate is accurately weighed in 50mL centrifuge tube, it is mixed that the rotation of the 5mL eddies of water is added
It is even, be added 25mL acetonitrile, concussion extract 15min, then plus 5gNaCl, 10mL n-hexane, shake 5min, 4000r/min centrifugation
5min takes acetonitrile layer into 100mL pear shape bottle, 40 DEG C of rotary evaporated to dryness；
1mL methanol-water (1:1) constant volume is added in pear shape bottle, be vortexed ultrasound, takes constant volume liquid into 2mL centrifuge tube, and 750 μ L second are added
Nitrile is saturated n-hexane, is vortexed, and 0.45 μm of organic phase, water phase filter membrane are crossed by high speed centrifugation Hou Qu lower layer, analyzes to HPLC-MS/MS.
2. measuring the remaining method of azithromycin in poultry livers tissue according to claim 1, it is characterised in that: described
It is as follows that HPLC-MS/MS detects azithromycin residual parameter:
Chromatographic parameter:
Chromatographic column: Agilent EclipsePlus C18 (1.8 μm of 2.1*150mm)；Column temperature: 40 DEG C；
Mobile phase: flow path AB: methanol；The aqueous formic acid of flow path BA:0.1%；
Flow velocity: 0.3mL/min, sample volume: 2 μ L；
Mass spectrometry parameters:
Type ion source: ESI (+)；
Nebulizing Gas Flow:3L/min；
Heating Gas:10L/min；
Interface Temperature:300 DEG C；
DLTemperature:250 DEG C；
Heat BlockTemperature:400 DEG C；
Drving Gas Flow:10L/min.
3. measuring the remaining method of azithromycin in poultry livers tissue according to claim 2, it is characterised in that: the stream
The gradient of dynamic phase are as follows:
。
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| PCT/CN2018/121217 WO2020118690A1 (en) | 2018-12-10 | 2018-12-14 | Method for measuring azithromycin residue in poultry liver tissue |
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| CN112362790A (en) * | 2020-11-26 | 2021-02-12 | 北京和合医学诊断技术股份有限公司 | Azithromycin detection method |
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