CN110057929A - The high-flux detection method of forbidden drug in a kind of feed and feed addictive - Google Patents
The high-flux detection method of forbidden drug in a kind of feed and feed addictive Download PDFInfo
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- CN110057929A CN110057929A CN201910205404.7A CN201910205404A CN110057929A CN 110057929 A CN110057929 A CN 110057929A CN 201910205404 A CN201910205404 A CN 201910205404A CN 110057929 A CN110057929 A CN 110057929A
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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
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- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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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
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- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The present invention relates to safety testing field, the high-flux detection method of forbidden drug in specially a kind of feed and feed addictive；First take extracting solution, extracting solution is passed through into the solid-phase extraction column after activation, eluent is collected, eluent is dried into progress membrane filtration after addition formic acid water-methanol solution is fully rotatable and obtains filtered fluid, filtered fluid is subjected to qualitative, quantitative determination using liquid chromatography-tandem mass spectrometry；A kind of high-flux detection method provided by the invention, reduces testing cost, improves detection efficiency, the residue detection of anti-microbial type and forbidden drug suitable for high-throughput feed.
Description
Technical field
The present invention relates to safety testing field, the high throughput of forbidden drug in specially a kind of feed and feed addictive
Detection method.
Background technique
Antibiotic serves not only as drug for preventing and treating bacterial infection disease in livestock and poultry breeding industry, can also make
Promote growth of animal to increase economic efficiency for feed addictive, thus is widely used in animal feed.However, in recent years
Food safety affair to be caused by feed constantly occurs, and a large amount of antibiotic are ingested after body, as blood circulation is distributed in
The organs such as lymph node, kidney and liver decline livestock and poultry immunity of organisms, and pathogen, which is taken advantage of a weak point, causes more serious harm, this
Outside, long-term excessive or improper can also cause bacterial drug resistance problem and in animal body residue problem using antibiotic.Antibiotic
After entering human body by food chain, serious harm will be constituted to human health.
Analysis method associated with the liquid chromatography mass of illegal addition forbidden drugs obtains in recent years in animal feed
It is more and more widely used, such as the detection of beta-receptor agonist, antibiotics and sedative, the inspection of part Common drugs
The respective country and professional standard of survey are also gradually put into effect.Have in reported document while detecting a kind of or several classes in food and resists
The method of mushroom and forbidden drug and antioxidant, but the method for lacking while detecting anti-microbial type and forbidden drug in feed.
Therefore, the detection method for needing to explore rapidly and efficiently separation detection multiclass anti-microbial type and forbidden drug at present, meets feed safety
The needs of detection fill up the blank of feed context of detection.
Summary of the invention
For the technical problem more than solving, the present invention provides a kind of high throughput of fresh milk multiple groups class residue of veterinary drug
Detection method；
The present invention is implemented as follows:
The high-flux detection method of forbidden drug, first takes extracting solution, extracting solution is led in a kind of feed and feed addictive
Solid-phase extraction column after overactivation collects eluent, eluent drying addition formic acid water-methanol solution is fully rotatable laggard
Row membrane filtration obtains filtered fluid, and filtered fluid is carried out qualitative, quantitative determination using liquid chromatography-tandem mass spectrometry.
Further, the extracting method of extracting solution includes: that acetonitrile solution is added in sample to be tested, described to be detected
The mass ratio of sample and the acetonitrile solution is 1:6, is mixed, and is vortexed, takes supernatant after centrifugation.
Further, the collection method of eluent is that the extracting solution is passed through PRIME with the flow velocity of every 3~4 seconds 1 drops
HLB solid-phase extraction column.
Further, the furnace drying method of eluent is to be dried up with 40~50 DEG C of nitrogen.
Further, acetonitrile solution is what acetonitrile was uniformly mixed with use for laboratory level-one water according to volume ratio 4:1
Drug solution.
Further, chromatographic condition are as follows: chromatographic column: 1.7 μm, 2.1*50mm；Flow velocity: 0.3ml/min；Sampling volume: 2 μ
l；Column temperature: 40 DEG C.
Further, mobile phase and degree elution time are as follows: mobile phase A: 0.1% aqueous formic acid；Mobile phase B: methanol；
0~3.0min of elution time, Mobile phase B is from 10% linear increase to 80%；3.0~4.0min of elution time, Mobile phase B are protected
Hold 80%；4.0~4.1min of elution time, Mobile phase B are down to 10% from 80%；4.1~5.0min of elution time, mobile phase
B keeps 10%.
Further, mobile phase and degree elution time are as follows: mobile phase A: water, Mobile phase B: methanol；Elution time is flowing
Phase B is from 10% linear increase to 80%；3.0~4.0min of elution time, Mobile phase B keep 80%；Elution time 4.0~
4.1min, Mobile phase B are down to 10% from 80%；4.1~5.0min of elution time, Mobile phase B keep 10%.
Further, Mass Spectrometry Conditions are as follows: ion source: electric spray ion source；Scanning mode: cation scanning；Detection side
Formula: multiple-reaction monitoring；Capillary voltage: 3.0KV；Ion source temperature: 150 DEG C；Desolvation temperature: 350 DEG C；Desolventizing gas
Flow: 800L/h.
Further, qualitativing quantitative measuring method includes: that the qualitative method goes out according to sample to be tested and standard substance
When peak is consistent, it is determined as target compound in conjunction with the qualitative and quota ion pair in mass spectrometry parameters；The quantitative approach is basis
Normal concentration and peak iso-surface patch standard working curve, bring equation into according to the peak area of the target compound in sample to be tested, count
Calculate the respective concentration of target compound；
The 227.1 and 140 monitoring ions as Clenbuterol are selected, are selected 277.1 and 168.1 as Clenbuterol
Quota ion；
The 302.2 and 164.1 monitoring ions as Ractopamine are selected, are selected 302.2 and 284.2 more as Lake
The quota ion pair of bar amine；
The 240.2 and 148.1 monitoring ion pairs as salbutamol are selected, are selected 240.0 and 222.1 as husky butylamine
The quota ion pair of alcohol；
251 and 92 are selected as the monitoring ion pair of sulphadiazine, selects 251 and 156 quota ion as sulphadiazine
It is right；
The 311.1 and 92 monitoring ion pairs as sulfadimethoxine are selected, are selected 311.1 and 156 as sulfanilamide (SN) two
The quota ion pair of Sulfamonomethoxine；
The 265.1 and 92 monitoring ion pairs as sulfamethyldiazine are selected, are selected 265.1 and 156 as methylene sulfonamide
The quota ion pair of pyrimidine；
The 281 and 91.8 monitoring ion pairs as 5-methoxysulfadiazine are selected, are selected 281 and 155.9 as sulfanilamide (SN) pair
The quota ion pair of Sulfamonomethoxine；
The 279.1 and 124.1 monitoring ion pairs as sulfadimidine are selected, are selected 279.1 and 186 as sulfanilamide (SN)
The quota ion pair of diformazan pyrimidine；
The 272.1 and 92 monitoring ion pairs as sulfamethizole are selected, are selected 272.1 and 156 as sulfamethizole
Quota ion pair；
The 254.1 and 92 monitoring ion pairs as sulfamethoxazole are selected, are selected 254.1 and 156 as sulfamethoxazole
Quota ion pair；
The 301.1 and 92.2 monitoring ion pairs as sulfaquinoxaline are selected, are selected 301.1 and 156.1 as sulfanilamide (SN) quinoline
Dislike the quota ion pair of quinoline；
The 332.1 and 288.1 monitoring ion pairs as Huang Bingsha star are selected, are selected 332.1 and 314.1 as Huang Bingsha
The quota ion pair of star；
The 358.2 and 96 monitoring ion pairs as Danofloxacin are selected, are selected 358.2 and 314.1 as Danofloxacin
Quota ion pair；
The 360.1 and 316.2 monitoring ion pairs as Enrofloxacin are selected, are selected 360.1 and 342.2 as En Nuosha
The quota ion pair of star；
Select the 385.9 and 299.1 monitoring ion pairs as sarafloxacin, select 385.9 and 342.1 as salad sand
The quota ion pair of star；
The 362 and 356.2 monitoring ion pairs as Difloxacin are selected, are selected 362 and 356.2 as Difloxacin
Quota ion pair；
The 334.1 and 233.2 monitoring ion pairs as pefloxacin are selected, are selected 334.1 and 290.6 husky as training fluorine
The quota ion pair of star；
The 320 and 276.2 monitoring ion pairs as Norfloxacin are selected, are selected 320 and 302.1 as Norfloxacin
Quota ion pair；
The 152.1 and 79.1 monitoring ion pairs as amantadine are selected, are selected 152.1 and 93.1 as amantadine
Quota ion pair；
The 180.2 and 81 monitoring ion pairs as Rimantadine are selected, are selected 180.2 and 163.2 as Rimantadine
Quota ion pair；
The 291.3 and 123 monitoring ion pairs as trimethoprim are selected, are selected 291.3 and 123 as trimethoprim
Quota ion pair；
The 749.5 and 158.2 monitoring ion pairs as azithromycin are selected, are selected 749.5 and 591.5 as Zitromax
The quota ion pair of element；
The 445 and 154 monitoring ion pairs as Doxycycline are selected, 445 and 428 quantifying as Doxycycline are selected
Ion pair；
The 264 and 77 monitoring ion pairs as olaquindox are selected, 264 and 103.9 quota ion as olaquindox is selected
It is right；
The 219 and 101.9 monitoring ion pairs as mequindox are selected, select 219 and 143 to determine as mequindox
Measure ion pair；
The 325 and 100 monitoring ion pairs as furaltadone are selected, select 325 and 281.1 to determine as furaltadone
Measure ion pair；
The 239 and 94.9 monitoring ion pairs as furantoin are selected, select 239 and 121.9 to determine as furantoin
Measure ion pair；
The 225.9 and 95 monitoring ion pairs as furazolidone are selected, select 225.9 and 122 to determine as furazolidone
Measure ion pair；
The 198.9 and 96.9 monitoring ion pairs as nitrofurazone are selected, are selected 198.9 and 125 as nitrofurazone
Quota ion pair；
The 437.3 and 361.2 monitoring ion pairs as dexamethasone are selected, 437.3 and 391.2 is selected as ground and fills in rice
The quota ion pair of pine；
The 407 and 55.1 monitoring ion pairs as lincomycin are selected, select 407 and 69.7 to determine as lincomycin
Measure ion pair；
The 869.4 and 174.2 monitoring ion pairs as Tilmicosin are selected, select 869.4 and 174.2 to examine as rice
The quota ion pair of star；
Select the 734.3 and 83 monitoring ion pairs as erythromycin, select 734.3 and 98 as erythromycin it is quantitative from
Son is right；
The 172 and 82 monitoring ion pairs as metronidazole are selected, 172 and 128 quota ion as metronidazole is selected
It is right；
Select the 142 and 81 monitoring ion pairs as Dimetridazole, select 142 and 96 as Dimetridazole it is quantitative from
Son is right；
Select 201 and 55 as Lip river nitre reach azoles monitoring ion pairs, select 201 and 140 as Lip river nitre reach azoles quantify from
Son is right；
The 321 and 152.2 monitoring ion pairs as chloramphenicol are selected, 321 and 152.2 quantifying as chloramphenicol are selected
Ion pair；
The 356 and 185 monitoring ion pairs as Florfenicol are selected, 356 and 227 quantifying as Florfenicol are selected
Ion pair.
Above scheme the utility model has the advantages that
A kind of high-flux detection method provided by the invention, reduces testing cost, improves detection efficiency, be suitable for
The residue detection of anti-microbial type and forbidden drug in high-throughput feed.
Specific embodiment
Technical solution of the present invention will be clearly and completely described below, it is clear that described embodiment is this
Invention a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
1. reagent and material
1.1 standard items
All kinds of antibiotic belong to illegal drug standard items in the present invention, and standard items are following:
Clenbuterol, Ractopamine, salbutamol, sulphadiazine, sulfadimethoxine, sulfamethyldiazine, sulphur
Amine is to Sulfamonomethoxine, sulfadimidine, sulfamethizole, sulfamethoxazole, sulfaquinoxaline, Ciprofloxacin, husky up to fluorine
Star, Enrofloxacin, sarafloxacin, Ofloxacin, Difloxacin, pefloxacin, Norfloxacin, amantadine, Rimantadine,
Trimethoprim, azithromycin, Doxycycline, olaquindox, mequindox, furaltadone, furantoin, furazolidone, furans west
Woods, dexamethasone, lincomycin, Tilmicosin, erythromycin, metronidazole, Dimetridazole, Lip river nitre reach azoles
1.2 reagent
Acetonitrile (Acetonitrile, 99.9%), methanol (Methanol, 99.9%), acetonitrile-aqueous solution, wherein second
Nitrile, methanol are chromatographic grade.
The preparation of acetonitrile-aqueous solution takes acetonitrile 80mL, water 20mL, mixes, obtains acetonitrile-aqueous solution.
1.3 standard solution are prepared
Appropriate standard items are accurately weighed respectively, are dissolved with acetonitrile, and it is molten to be configured to the standard inventory that concentration is 100 μ g/mL
Liquid, -18 DEG C of freezings are kept in dark place.
Intermediate standard solution is prepared: it is pipetted in 1mL Standard Stock solutions (4.5) and 10mL volumetric flask respectively, it is fixed with acetonitrile
Hold the intermediate standard solution for being configured to that concentration is 10 μ g/mL to scale, 0 DEG C~4 DEG C refrigerations are kept in dark place.
1.4 solid-phase extraction column
Solid-phase extraction column PRIME HLB, specification 6CC, 200mg.
Embodiment one
The foundation of the high-flux detection method of forbidden drug in feed and feed addictive
2. experimental method
2.1 sample extractions and purification
5g sample is weighed in 50mL centrifuge tube, adds acetonitrile solution 15ml, is sufficiently mixed, be vortexed, 10000r/min from
Heart 5min.
Above-mentioned supernatant 5ml is taken, PRIME HLB solid-phase extraction column is passed through with the flow velocity of every 3~4 seconds 1 drops.Collect elution
Liquid 4ml, 40 DEG C are dried with nitrogen addition 1.00ml0.2% formic acid water-methanol (1:1) solution, sufficient vortex, with 0.2 μm of filter membrane mistake
Filter, filtrate measure for high performance liquid chromatography-tandem mass instrument.
2.2 chromatographic condition
A group chromatographic column: BEH C18 column, 2.1 × 50mm, 1.7 μm；Column temperature: 40 DEG C；Sample volume: 2 μ L；Mobile phase: A:
0.1% aqueous formic acid, wherein aqueous formic acid contains the ammonium acetate of 5mmol/L；Mobile phase B: methanol；Flow velocity: 0.30mL/
min；Gradient: 0~1.0min, 90%A, 1.0~3.0min, 20%A, 3.0~4.0min, 20%, 4.0~
5.0min, 90%A.
B group chromatographic column: BEH C18 column, 2.1 × 50mm, 1.7 μm；Column temperature: 40 DEG C；Sample volume: 2 μ L；Mobile phase: A:
Water；B: methanol；Flow velocity: 0.30mL/min；Gradient: 0~1.0min, 90%A, 1.0~3.0min, 20%A, 3.0~
4.0min, 20%, 4.0~4.1min, 90%A, 4.1~5.0min, 90%A.
2.3 Mass Spectrometry Conditions
A group Mass Spectrometry Conditions: ionization mode: ESI+；Capillary voltage: 3.0KV；Orifice potential: 25~90V；Remove solvent
Temperature: 350 DEG C；Go solvent stream fast: 800L/h；Carrier gas, High Purity Nitrogen (> 99.999%).
B group Mass Spectrometry Conditions: ionization mode: Negative electrospray ionization；Capillary voltage: 2.0kV；Ion source temperature: 150 DEG C；
Remove solvent temperature: 350 DEG C；Carrier gas, High Purity Nitrogen (> 99.999%).
Detection mode: multiple-reaction monitoring
3. qualitative, quota ion condition
3.1.A qualitative, quota ion pair is organized
Table one, A group is qualitative, quota ion pair table
3.2.B qualitative, quota ion pair is organized
Table two, B group is qualitative, quota ion pair table
4. qualitative method
Pass through the retention time of sample chromatogram and retention time, the feature of each chromatographic peak of respective standard standard solution
The characteristic ion of ion and each chromatographic peak of respective concentration standard solution contrasts qualitative.Sample and standard solution retention time
Relative deviation is not more than 1.5%；The relative ion abundance of sample characteristics example and the relative ion abundance of standard solution are consistent,
Relative ion abundance deviation is provided no more than table three, then can determine whether the presence of component to be measured in sample.
Table three, the maximum allowable offset table of relative ion abundance
5. quantitative approach
It materialses solution, machine measurement on standard solution, quantified by external standard method, peak area Ying Yi in standard solution and sample
In the range of linearity of device detection.
6. result calculates
With the external standard method in data processing software, or drafting standard curve, residual quantity in sample is calculated according to formula (1)
In formula:
X --- the content of the component to be measured in sample, unit are milligrams per kilogram (mg/kg)；
C --- the concentration of component to be measured in the sample liquid as obtained by standard curve, unit are nanograms per milliliter (ng/mL)；
V --- the final constant volume of sample liquid, unit are milliliter (mL)；
M --- sample sample weighting amount, unit are gram (g).
Claims (10)
1. the high-flux detection method of forbidden drug in a kind of feed and feed addictive, which is characterized in that extracting solution is first taken, it will
Extracting solution collects eluent by the solid-phase extraction column after activation, and eluent is dried addition formic acid water-methanol solution and is sufficiently revolved
Membrane filtration is carried out after turning and obtains filtered fluid, and filtered fluid is subjected to qualitative, quantitative determination using liquid chromatography-tandem mass spectrometry.
2. the high-flux detection method of forbidden drug, feature exist in feed according to claim 1 and feed addictive
In the extracting method of the extracting solution includes: that acetonitrile solution, the sample to be tested and the second is added in sample to be tested
The mass ratio of nitrile aqueous solution is 1:6, is mixed, and is vortexed, takes supernatant after centrifugation.
3. the high-flux detection method of forbidden drug, feature exist in feed according to claim 1 and feed addictive
In the collection method of the eluent is that the extracting solution is passed through PRIME HLB Solid Phase Extraction with the flow velocity of every 3~4 seconds 1 drops
Column.
4. the high-flux detection method of forbidden drug, feature exist in feed according to claim 1 and feed addictive
In the furnace drying method of the eluent is to be dried up with 40~50 DEG C of nitrogen.
5. the high-flux detection method of forbidden drug, feature exist in feed according to claim 2 and feed addictive
In the acetonitrile solution is the drug solution that acetonitrile is uniformly mixed with use for laboratory level-one water according to volume ratio 4:1.
6. the high-flux detection method of forbidden drug, feature exist in feed according to claim 1 and feed addictive
In the chromatographic condition are as follows: chromatographic column: 1.7 μm, 2.1*50mm；Flow velocity: 0.3ml/min；Sampling volume: 2 μ l；Column temperature: 40
℃。
7. the high-flux detection method of forbidden drug, feature exist in feed according to claim 1 and feed addictive
In the mobile phase and degree elution time are as follows: mobile phase A: 0.1% aqueous formic acid；Mobile phase B: methanol；Elution time 0~
3.0min, Mobile phase B is from 10% linear increase to 80%；3.0~4.0min of elution time, Mobile phase B keep 80%；When elution
Between 4.0~4.1min, Mobile phase B is down to 10% from 80%；4.1~5.0min of elution time, Mobile phase B keep 10%.
8. the high-flux detection method of forbidden drug, feature exist in feed according to claim 1 and feed addictive
In the mobile phase and degree elution time are as follows: mobile phase A: water, Mobile phase B: methanol；Elution time is Mobile phase B from 10% line
Property rises to 80%；3.0~4.0min of elution time, Mobile phase B keep 80%；4.0~4.1min of elution time, Mobile phase B
10% is down to from 80%；4.1~5.0min of elution time, Mobile phase B keep 10%.
9. the high-flux detection method of forbidden drug, feature exist in feed according to claim 1 and feed addictive
In Mass Spectrometry Conditions are as follows: ion source: electric spray ion source；Scanning mode: cation scanning；Detection mode: multiple-reaction monitoring；Hair
Tubule voltage: 3.0KV；Ion source temperature: 150 DEG C；Desolvation temperature: 350 DEG C；Desolventizing gas flow: 800L/h.
10. the high-flux detection method of forbidden drug, feature exist in feed according to claim 1 and feed addictive
In, when the qualitativing quantitative measuring method includes: that the qualitative method is consistent with standard substance appearance according to sample to be tested,
It is determined as target compound in conjunction with the qualitative and quota ion pair in mass spectrometry parameters；The quantitative approach be according to normal concentration with
Peak iso-surface patch standard working curve brings equation into according to the peak area of the target compound in sample to be tested, calculates target chemical combination
The respective concentration of object；The 227.1 and 140 monitoring ions as Clenbuterol are selected, are selected 277.1 and 168.1 as Ke Lunte
The quota ion of sieve；The 302.2 and 164.1 monitoring ions as Ractopamine are selected, are selected 302.2 and 284.2 as Lay
The quota ion pair of gram dopamine；The 240.2 and 148.1 monitoring ion pairs as salbutamol are selected, 240.0 Hes are selected
222.1 quota ion pair as salbutamol；251 and 92 are selected as the monitoring ion pair of sulphadiazine, selects 251 and 156
Quota ion pair as sulphadiazine；The 311.1 and 92 monitoring ion pairs as sulfadimethoxine are selected, are selected
311.1 and 156 quota ion pair as sulfadimethoxine；Select 265.1 and 92 monitoring as sulfamethyldiazine
Ion pair selects 265.1 and 156 quota ion pair as sulfamethyldiazine；Select 281 and 91.8 as sulfanilamide (SN) to methoxy
The monitoring ion pair of pyrimidine selects 281 and 155.9 quota ion pair as 5-methoxysulfadiazine；Select 279.1 Hes
The 124.1 monitoring ion pair as sulfadimidine selects 279.1 and 186 quota ion pair as sulfadimidine；
Select the 272.1 and 92 monitoring ion pairs as sulfamethizole, select 272.1 and 156 as sulfamethizole it is quantitative from
Son is right；The 254.1 and 92 monitoring ion pairs as sulfamethoxazole are selected, select 254.1 and 156 to determine as sulfamethoxazole
Measure ion pair；The 301.1 and 92.2 monitoring ion pairs as sulfaquinoxaline are selected, are selected 301.1 and 156.1 as sulfanilamide (SN) quinoline
Dislike the quota ion pair of quinoline；The 332.1 and 288.1 monitoring ion pairs as Huang Bingsha star are selected, select 332.1 and 314.1 to make
For the quota ion pair of Huang Bingsha star；The 358.2 and 96 monitoring ion pairs as Danofloxacin are selected, select 358.2 and 314.1
Quota ion pair as Danofloxacin；The 360.1 and 316.2 monitoring ion pairs as Enrofloxacin are selected, 360.1 Hes are selected
342.2 quota ion pair as Enrofloxacin；The 385.9 and 299.1 monitoring ion pairs as sarafloxacin are selected, are selected
385.9 and 342.1 quota ion pair as sarafloxacin；The 362 and 356.2 monitoring ion pairs as Difloxacin are selected,
Select 362 and 356.2 quota ion pair as Difloxacin；Select the 334.1 and 233.2 monitoring ions as pefloxacin
It is right, select 334.1 and 290.6 quota ion pair as pefloxacin；Select 320 and 276.2 monitoring as Norfloxacin
Ion pair selects 320 and 302.1 quota ion pair as Norfloxacin；Select 152.1 and 79.1 prison as amantadine
Measured ion pair selects 152.1 and 93.1 quota ion pair as amantadine；It selects 180.2 and 81 as Rimantadine
Ion pair is monitored, 180.2 and 163.2 quota ion pair as Rimantadine is selected；It selects 291.3 and 123 as methoxy benzyl
The monitoring ion pair of pyridine selects 291.3 and 123 quota ion pair as trimethoprim；Select 749.5 and 158.2 as Ah
The monitoring ion pair of miramycin selects 749.5 and 591.5 quota ion pair as azithromycin；Select 445 and 154 as
The monitoring ion pair of Doxycycline selects 445 and 428 quota ion pair as Doxycycline；It selects 264 and 77 as quinoline second
The monitoring ion pair of alcohol selects 264 and 103.9 quota ion pair as olaquindox；It selects 219 and 101.9 as acetyl first
The monitoring ion pair of quinoline selects 219 and 143 quota ion pair as mequindox；It selects 325 and 100 as furaltadone
Monitoring ion pair, select 325 and 281.1 quota ion pair as furaltadone；It selects 239 and 94.9 as furantoin
Monitoring ion pair, select 239 and 121.9 quota ion pair as furantoin；It selects 225.9 and 95 as furazolidone
Monitoring ion pair, select 225.9 and 122 quota ion pair as furazolidone；Select 198.9 and 96.9 as furans west
The monitoring ion pair of woods selects 198.9 and 125 quota ion pair as nitrofurazone；Select 437.3 and 361.2 as ground
The monitoring ion pair of Sai meter Song selects 437.3 and 391.2 quota ion pair as dexamethasone；Select 407 and 55.1 as
The monitoring ion pair of lincomycin selects 407 and 69.7 quota ion pair as lincomycin；Selection 869.4 and 174.2 is made
For the monitoring ion pair of Tilmicosin, 869.4 and 174.2 quota ion pair as Tilmicosin is selected；Selection 734.3 and 83
As the monitoring ion pair of erythromycin, 734.3 and 98 quota ion pair as erythromycin is selected；It selects 172 and 82 as first
The monitoring ion pair of nitre azoles selects 172 and 128 quota ion pair as metronidazole；It selects 142 and 81 as Dimetridazole
Ion pair is monitored, 142 and 96 quota ion pair as Dimetridazole is selected；Select 201 and 55 monitorings that azoles is reached as Lip river nitre
Ion pair selects 201 and 140 quota ion pairs that azoles is reached as Lip river nitre；Select 321 and 152.2 as chloramphenicol monitoring from
Son is right, selects 321 and 152.2 quota ion pair as chloramphenicol；Select the 356 and 185 monitoring ions as Florfenicol
It is right, select 356 and 227 quota ion pair as Florfenicol.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112782405A (en) * | 2020-12-25 | 2021-05-11 | 石家庄四药有限公司 | Detection method for antioxidant degradation product in levofloxacin lactate and sodium chloride injection |
| CN114539170A (en) * | 2021-12-31 | 2022-05-27 | 华南农业大学 | Hapten and artificial antigen for simultaneously detecting amantadine, olaquindox and chloramphenicol and preparation method and application thereof |
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2019
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112782405A (en) * | 2020-12-25 | 2021-05-11 | 石家庄四药有限公司 | Detection method for antioxidant degradation product in levofloxacin lactate and sodium chloride injection |
| CN114539170A (en) * | 2021-12-31 | 2022-05-27 | 华南农业大学 | Hapten and artificial antigen for simultaneously detecting amantadine, olaquindox and chloramphenicol and preparation method and application thereof |
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Application publication date: 20190726 |