CN105548392A - Method for simultaneously detecting various antibiotics in livestock and poultry manure by high performance liquid chromatography - Google Patents
Method for simultaneously detecting various antibiotics in livestock and poultry manure by high performance liquid chromatography Download PDFInfo
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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
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Abstract
The invention relates to an antibiotic detection method, and in particular, relates to a method for simultaneously detecting various antibiotics in livestock and poultry manure by high performance liquid chromatography; the method comprises the steps: pretreating a livestock and poultry manure sample, to obtain a to-be-detected liquid; performing analyte separation of the to-be-detected liquid by a high performance liquid chromatograph, and calculating peak areas corresponding to separated residual antibiotics; and quantitatively calculating according to a standard curve, to obtain the residual content. The method is applied in detection of 11 kinds of residual antibiotics in the livestock and poultry manure; compared with a high performance liquid chromatography-mass spectrometry coupled technique, the method has the advantages of lower detection cost and high detection efficiency, can simultaneously separate 11 kinds of antibiotics, has analytes without interference of major interferents, and basically does not affect qualitative and quantitative analysis of the analytes.
Description
Technical field
The present invention relates to a kind of microbiotic detection method, be specially the method utilizing high performance liquid chromatography simultaneously to detect Multiple Classes of Antibiotics in feces of livestock and poultry.
Background technology
Microbiotic refers to the same or similar material having killing or suppress pathogenic microorganism of structure that is that obtained through cultivation by microorganisms such as bacterium, actinomyces, fungies or that synthesize by chemical synthesis.Microbiotic a large amount of is in recent years widely used in livestock and poultry breeding industry as veterinary drug and feed addictive, in animal diseases control, raising feed efficiency, promotes to play an important role in animal growth.But the microbiotic entered in animal body by oral or intramuscular injection can not be completely absorbed utilization, account for 40%-90% of dosage with the form of original shape or metabolite with the amount of urinating or ight soil excretes.Therefore, veterinary antibiotic very easily enters in the environment such as agricultural land soil along with fecaluria etc., causes the Spreading and diffusion of environment antibiotic residue and drug-resistant bacteria, has a strong impact on the safety of whole Agro-ecological System, finally jeopardizes human health.The while of foundation, in testing environment medium, the analytical approach of Multiple Classes of Antibiotics is the basis of its environmental behaviour of research and Ecological Environment Risk.
The microbiotic of Environmental Residues belongs to trace materials, existing method many employings high performance liquid chromatograph-mass spectrometric hyphenated technique is studied, but this technical costs is relatively high, focus mostly in animal food field to the detect delay of veterinary antibiotic residual quantity at present, and the Antibiotics detected is single, know and enter multiple antibiotic residues amount in the feces of livestock and poultry of farm environment, to guaranteeing that ecological environment security is significant.
Summary of the invention
In order to the microbiotic detection method cost overcoming above-mentioned prior art is high, detection of antibiotics kind is few and the shortcoming resting on animal food detection field with not enough, the invention provides a kind of method utilizing high performance liquid chromatography to detect multiple veterinary antibiotic fast.
The present invention is platform with high performance liquid chromatograph, establishes the detection method of multiple antibiotic residues in feces of livestock and poultry, and the method simultaneously detecting multiple veterinary antibiotic is detecting the application in ecologic environment residual antibiotic.Particularly be applied to and detect 11 kinds of microbiotic residual in feces of livestock and poultry.
Object of the present invention is realized by following proposal:
Utilize high performance liquid chromatography to detect the method for Multiple Classes of Antibiotics in feces of livestock and poultry simultaneously, comprise following steps:
(1) pre-service is carried out to feces of livestock and poultry sample, obtain liquid to be measured;
By after the feces of livestock and poultry sample freeze drying that gathers back, extract with EDTA-Mcllvaine damping fluid and organic mixing extraction agent, normal hexane degrease first used by extract, then the HLB pillar after overactivation carries out enrichment: remove partial impurities with 25% methanol solution drip washing HLB pillar, and drain 5min, then use the HLB pillar of 65% methanol solution wash-out enrichment, eluent revolves steaming and dries up, be settled to 1mL mutually by initial flow, cross 0.22 μm of film, obtain liquid to be measured;
EDTA-Mcllvaine buffer method used is: and Na
2hPO
4the solution being mixed with 0.1mol/L citric acid solution and 0.2mol/L respectively, according to volume ratio 8:5 mixing, is mixed with Mcllvaine solution; Get the Na of 37.2g
2-EDTA, with Mcllvaine solution, joins to obtain 0.1mol/LEDTA-Mcllvaine extract, is adjusted to pH=4.0 with HCl or NaOH;
Organic mixing extraction agent used is methyl alcohol: acetonitrile: acetone, according to volume ratio 2:2:1 mixing, uses H
3pO
4pH is regulated to be 4.
(2) liquid to be measured is carried out by high performance liquid chromatograph the separation analyzing thing;
Liquid to be measured is carried out by high performance liquid chromatograph the separation analyzing thing, and the chromatographic condition of mensuration is:
Adopt AgilentEclipsePlusC18 chromatographic column: 150mm × 4.6mm, 3.5 μm, Agilent company; Binary gradient pump; Variable wavelength scanning UV-detector; Mobile phase A is 0.1% formic acid solution, and Mobile phase B is that methyl alcohol and acetonitrile are according to volume ratio 1:1; Flow velocity is 0.6mL/min; Sampling volume 20 μ L; Column temperature 35 DEG C; Determined wavelength is 274nm; Gradient elution order: 0 ~ 18min, 80%A; 18 ~ 20min, 80% ~ 40%A; 20 ~ 30min, 40%A; 30 ~ 32min, 40% ~ 80%A; 32 ~ 35min, 80%A.
(3) calculate peak area corresponding to isolated residual antibiotic, quantitatively calculate according to typical curve, draw residual content;
Described typical curve, according to step (1), step (2), adopts identical reagent and parameter, draws under same experimental conditions.
The method is used for detecting 11 kinds of microbiotic simultaneously, comprises terramycin (OTC), aureomycin (CTC), sulfadimidine (SDMe), sulfamethoxazole (SMZ), sulphathiazole (ST), daimeton (SMN), Ciprofloxacin (CIP), Norfloxacin (NOR), Enrofloxacin (ENR), tylosin (TYL), chloromycetin (CAP).
The method utilizing high performance liquid chromatography simultaneously to detect Multiple Classes of Antibiotics provided by the invention, be applied to the detection of 11 kinds of residual antibiotics in feces of livestock and poultry, 11 kinds of target microbiotic all have good absorption under high performance liquid chromatograph UV-detector 274nm wavelength, Detection results is best, by the optimal combination to conditions such as mobile phase and each component proportion, flow velocity, temperature, determine the top condition that 11 kinds of target microbiotic detect simultaneously.Compared with high performance liquid chromatograph-mass spectrometric hyphenated technique, testing cost is lower; Detection efficiency is high, can be separated 11 kinds of microbiotic simultaneously; Analyze thing to disturb without main chaff interference, not impact analysis thing quantitative and qualitative analysis substantially.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Utilize high performance liquid chromatography to detect the instrument condition of the method for Multiple Classes of Antibiotics in feces of livestock and poultry as follows simultaneously:
Detecting device is variable wavelength scanning UV-detector and VWD, and determined wavelength is 274nm, column temperature 35 DEG C, flow velocity is 0.6mL/min, sampling volume 20 μ L, and mobile phase A is 0.1% formic acid solution, Mobile phase B is methyl alcohol/acetonitrile is 1:1 mixing according to v/v, gradient elution order: 0 ~ 18min, 80%A; 18 ~ 20min, 80% ~ 40%A; 20 ~ 30min, 40%A; 30 ~ 32min, 40% ~ 80%A; 32 ~ 35min, 80%A.
The separating monitoring of 11 kinds of antibiotic residues in pig manure:
(1) instrument is U.S.'s Agilent 1200 high performance liquid chromatograph, chromatographic column specification is AgilentEclipsePlusC18 (150mm × 4.6mm, 3.5 μm), variable wavelength scanning UV-detector (VWD), determined wavelength 274nm, column temperature 35 DEG C, flow velocity is 0.6mL/min, sampling volume 20 μ L, mobile phase A is 0.1% formic acid solution, Mobile phase B is methyl alcohol/acetonitrile is 1:1 mixing according to v/v, gradient elution order: 0 ~ 18min, 80%A; 18 ~ 20min, 80% ~ 40%A; 20 ~ 30min, 40%A; 30 ~ 32min, 40% ~ 80%A; 32 ~ 35min, 80%A.Agilent1200LC workstation.
(2) mensuration of typical curve: accurately take 11 kinds of each 10mg of target microbiotic standard items in the brown volumetric flask of 10mL, Norfloxacin 0.03mol/LNaOH dissolves and is settled to 10mL, all the other 10 kinds of microbiotic objects methyl alcohol dissolves and constant volume, be mixed with that 1mg/mL is mono-marks storing solution, keep in Dark Place in 4 DEG C.Accurately pipette various list and mark storing solution, with brown volumetric flask prepare 11 kinds of antibiotic concentrations be 0.05,0.1,0.5,1.0,5.0,10.0,50.0, the mixed standard solution of 100mg/L, adopt the condition of step (1) to test, obtain working curve.11 kinds of antibiotic linear relationships, related coefficient and detection limits are in table 1.
(3) activation of HLB pillar: HLB pillar before use, successively activates with 5mL methyl alcohol, 10mL pure water.
(4) pre-service of feces of livestock and poultry sample and test: by the pig manure sample gathered back, test specimen selects bio-farm, Shouyang County, Shanxi Province one, microbiotic is not used in breeding process, after testing not containing microbiotic object, freeze drying, ground 2mm sieve, accurately take 1.0g ground sample, 11 kinds of microbiotic are mixed in pig manure and obtain mixing pig manure sample, first 10mLEDTA-Mcllvaine damping fluid vortex mixing 30s is added, the ultrasonic 15min of normal temperature, the centrifugal 15min of 8000r/min at 4 DEG C, supernatant is transferred in other brown container, repeat to extract once, extraction is repeated twice again with the organic mixed extract of 5mL, step is the same.
Merge extract, after adding 10mL normal hexane degrease, cross 0.45 μm of filter membrane, Rotary Evaporators is used to be concentrated into 3-5mL extract after mistake film, extract after concentrated is with the HLB post after 1mL/min flow velocity overactivation, be 25:75 mixed liquor drip washing HLB pillar with the first alcohol and water v/v of 5mL, and drain 5min, be 65:35 mixed liquor wash-out target microbiotic with the first alcohol and water v/v of 10mL, collect eluent, be concentrated into dry on Rotary Evaporators, 1mL is settled to mutually by initial flow, cross 0.22 μm of film, upper machine is to be measured, high performance liquid chromatography discrete testing is carried out according to the condition of step (1).
(5) to the tracing analysis that above-mentioned test obtains, carry out integration to isolated residual target microbiotic area, the typical curve that establishing criteria product make quantitatively calculates, and draws residual content, and calculate the recovery, TIANZHU XINGNAO Capsul is in table 2.
Table 1 UV-detector lower 11 kinds of microbiotic linear relationships, related coefficient and detection limits
The antibiotic recovery of table 211 kind of target, standard deviation, detection limit and quantitative limit
Note: ST-sulphathiazole; CIP-Ciprofloxacin; OTC-terramycin; NOR-Norfloxacin; SDMe-sulfadimidine; ENR-Enrofloxacin; SMN-daimeton; SMZ-sulfamethoxazole; CTC-aureomycin; CAP-chloromycetin; TYL-tylosin.
Claims (3)
1. utilize high performance liquid chromatography to detect the method for Multiple Classes of Antibiotics in feces of livestock and poultry simultaneously, it is characterized in that, comprise following steps:
(1) pre-service is carried out to feces of livestock and poultry sample, obtain liquid to be measured;
By after the feces of livestock and poultry sample freeze drying that gathers back, extract with EDTA-Mcllvaine damping fluid and organic mixing extraction agent, normal hexane degrease first used by extract, then the HLB pillar after overactivation carries out enrichment: remove partial impurities with 25% methanol solution drip washing HLB pillar, and drain 5min, then use the HLB pillar of 65% methanol solution wash-out enrichment, eluent revolves steaming and dries up, be settled to 1mL mutually by initial flow, cross 0.22 μm of film, obtain liquid to be measured;
(2) liquid to be measured is carried out by high performance liquid chromatograph the separation analyzing thing;
Liquid to be measured is carried out by high performance liquid chromatograph the separation analyzing thing, and the chromatographic condition of mensuration is:
Adopt AgilentEclipsePlusC18 chromatographic column: 150mm × 4.6mm, 3.5 μm, Agilent company; Binary gradient pump; Variable wavelength scanning UV-detector; Mobile phase A is 0.1% formic acid solution, and Mobile phase B is that methyl alcohol and acetonitrile are according to volume ratio 1:1; Flow velocity is 0.6mL/min; Sampling volume 20 μ L; Column temperature 35 DEG C; Determined wavelength is 274nm; Gradient elution order: 0 ~ 18min, 80%A; 18 ~ 20min, 80% ~ 40%A; 20 ~ 30min, 40%A; 30 ~ 32min, 40% ~ 80%A; 32 ~ 35min, 80%A;
(3) calculate peak area corresponding to isolated residual antibiotic, quantitatively calculate according to typical curve, draw residual content;
Described typical curve, according to step (1), step (2), adopts identical reagent and parameter, draws under same experimental conditions.
2. the method utilizing high performance liquid chromatography simultaneously to detect Multiple Classes of Antibiotics according to claim 1, is characterized in that, the EDTA-Mcllvaine buffer method described in step (1) is: and Na
2hPO
4the solution being mixed with 0.1mol/L citric acid solution and 0.2mol/L respectively, according to volume ratio 8:5 mixing, is mixed with Mcllvaine solution; Get the Na of 37.2g
2-EDTA, with Mcllvaine solution, joins to obtain 0.1mol/LEDTA-Mcllvaine extract, is adjusted to pH=4.0 with HCl or NaOH;
Described organic mixing extraction agent is methyl alcohol: acetonitrile: acetone, according to volume ratio 2:2:1 mixing, uses H
3pO
4pH is regulated to be 4.
3. the method utilizing high performance liquid chromatography simultaneously to detect Multiple Classes of Antibiotics according to claim 1 and 2, it is characterized in that, the method is used for detecting 11 kinds of microbiotic simultaneously, comprises terramycin, aureomycin, sulfadimidine, sulfamethoxazole, sulphathiazole, daimeton, Ciprofloxacin, Norfloxacin, Enrofloxacin, tylosin, chloromycetin.
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Cited By (6)
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| CN106124683A (en) * | 2016-08-26 | 2016-11-16 | 中国兽医药品监察所 | A kind of method of multiple antimicrobial component in veterinary drug of detection simultaneously |
| CN106596780A (en) * | 2016-12-21 | 2017-04-26 | 南京大学 | Method for detecting contents of various antibiotics in water by combined use of high pressure liquid chromatography and mass spectrum |
| CN107490649A (en) * | 2017-09-15 | 2017-12-19 | 河南省兽药饲料监察所 | The screening method of 62 kinds of antibacterials in a kind of farm animal excrement |
| CN109633065A (en) * | 2018-12-28 | 2019-04-16 | 沈阳出入境检验检疫局检验检疫综合技术中心 | The detection method of medicament residue in a kind of animal body |
| CN109946392A (en) * | 2019-03-06 | 2019-06-28 | 江西省农业科学院畜牧兽医研究所 | A kind of method of Ciprofloxacin in detection feces of livestock and poultry |
| CN112763610A (en) * | 2020-12-28 | 2021-05-07 | 浙江大学 | Method for detecting antibiotics in soil |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106124683A (en) * | 2016-08-26 | 2016-11-16 | 中国兽医药品监察所 | A kind of method of multiple antimicrobial component in veterinary drug of detection simultaneously |
| CN106596780A (en) * | 2016-12-21 | 2017-04-26 | 南京大学 | Method for detecting contents of various antibiotics in water by combined use of high pressure liquid chromatography and mass spectrum |
| CN106596780B (en) * | 2016-12-21 | 2019-06-25 | 南京大学 | The method of Multiple Classes of Antibiotics content in high pressure liquid chromatography-mass spectrometry detection water |
| CN107490649A (en) * | 2017-09-15 | 2017-12-19 | 河南省兽药饲料监察所 | The screening method of 62 kinds of antibacterials in a kind of farm animal excrement |
| CN109633065A (en) * | 2018-12-28 | 2019-04-16 | 沈阳出入境检验检疫局检验检疫综合技术中心 | The detection method of medicament residue in a kind of animal body |
| CN109946392A (en) * | 2019-03-06 | 2019-06-28 | 江西省农业科学院畜牧兽医研究所 | A kind of method of Ciprofloxacin in detection feces of livestock and poultry |
| CN112763610A (en) * | 2020-12-28 | 2021-05-07 | 浙江大学 | Method for detecting antibiotics in soil |
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