CN105259277A - Method for detecting residual quantity of 18 sulfanilamide drugs in beef and mutton - Google Patents
Method for detecting residual quantity of 18 sulfanilamide drugs in beef and mutton Download PDFInfo
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Abstract
The invention discloses a method for detecting residual quantity of 18 sulfanilamide drugs in beef and mutton. The method comprises taking 5g of uniform beef and mutton, adding anhydrous magnesium sulfate, sodium acetate and acetonitrile acetate solutions into the beef and mutton, carrying out high-speed homogenized extraction, carrying out centrifugation, carrying out vortex mixing purification impurity-removal on the supernatant by an adsorbent containing a plurality of purification materials, carrying out pressure reduction or nitrogen blowing condensation on the supernatant subjected to re-centrifugation until drying, redissolving the residues, after shaking-up, filtering the solution by a microfiltration membrane with pore sizes of 0.22 micrometers to obtain a sample solution, carrying out separation by a reversed phase column filled with C18 as a filler, carrying out ultraviolet light on-line rapid derivation, carrying out detection by a fluorescence detector, carrying out qualitative analysis according chromatographic peak retention time, carrying out quantification by an external standard method and calculating residual quantity of 18 sulfanilamide drugs in beef and mutton. The method has simple processes, utilizes less amount of a reagent, has high detection sensitivity, releases simultaneous rapid detection of 18 sulfanilamide drugs by one step, greatly shortens analysis time and has a good application prospect.
Description
Technical field
The present invention relates to technical field of food safety detection, specifically the detection method of 18 kinds of sulfa antibiotics residual quantities in a kind of ox or sheep musculature.
Background technology
Beef and mutton are the meat products that consumption figure is large, and it is nutritious, are rich in the various trace elements such as protein, fat, phosphatide, multivitamin, mineral matter and calcium, phosphorus, iron, zinc, copper, manganese.Beef and mutton is of high nutritive value, and is the important sources of human nutrition, is also large consumption of meat product.
Sulfa drugs is a class microbiotic with P-aminobenzene-sulfonamide structure of Prof. Du Yucang, because of its has a broad antifungal spectrum, inexpensive, easy to use and be widely used in livestock breed aquatics.But the Use out of range of sulfanilamide (SN), can at animal body accumulations such as cattle and sheep, and accumulate in human body by food such as beef and mutton, the potential resistance to the action of a drug, teratogenesis, the harm such as carcinogenic are caused to human body.At present, China and the most countries such as the U.S., European Union all have clear stipulaties to the most high residue amount of sulfa drugs in food.
At present, in food, the detection method of sulfa drug residue mainly contains: microbiological method, spectrophotometric method, immunoassay, molecular imprinting analytic approach, capillary electrophoresis, chromatographic technique and coupling technique etc.Microbial method and spectrophotometric method simple to operate, cheap, but the accuracy of result and sensitivity are not high, can not meet the testing requirement of actual sample; Immunoassay comprises radioimmunoassay technique, Enzyme-multiplied immune technique, fluorescence immunoassay technology and biosensor technique, immunoassay and molecular imprinting analytic approach all have applied widely, highly sensitive, the advantage that accuracy is high, but the ability detecting multi-medicament residual is weak, and accurate quantitative analysis ability is weak simultaneously.In recent years, capillary electrophoresis technique is used widely, but due to its sample size few, sensitivity is restricted, and can not be used for the detection of trace materials.Chromatographic technique mainly contains high performance liquid chromatography, vapor-phase chromatography, thin-layered chromatography and immunochromatography, and coupling technique is HPLC MS and gas chromatography-mass spectrography mainly.It is high that above-mentioned chromatographic technique all has resolution, the advantages such as detectability is low, wherein high performance liquid chromatography and HPLC MS apply maximum detection methods in sulfa drugs analysis, but because mass spectroscopy instrument is expensive, and it is high to testing requirement, during high performance liquid chromatography employing UV-detector, sensitivity is low, poor selectivity.
Pre-treating method directly affects accuracy and the sensitivity of detection method, sulfa drugs pre-treating method respectively has its relative merits, wherein QuEChERS is as a kind of quick, simple, cheap, efficient, durable and safe sample treatment, be used widely in each field, but because the method for original European Union and AOAC is mainly for the detection of fruit, pesticide residues in vegetables medicine, and meat matrix more complicated, creationary transformation need be carried out to original formula and be suitable for just now.
The sulfa antibiotics existed in food belongs to trace materials, and developed country's many employings high performance liquid chromatograph-mass spectrometric hyphenated technique detects, and the method qualitative, quantitative is all very accurate, but cost is relatively high, has promoted the use of certain limitation in China.
Sulfa drugs itself does not fluoresce, and just can only can make it have fluorescent characteristic by derivative mode.Sulfanilamide (SN) contains photochemical activity group, photochemical reaction can occur, and produces fluorescent material, thus using fluorescence detecting device direct-detection.
Summary of the invention
The shortcomings such as sulfa antibiotics detection method cost in above-mentioned prior art is high in order to overcome, complex steps, with not enough, the object of the present invention is to provide the detection method of 18 kinds of sulfa antibiotics in a kind of beef and mutton.
For achieving the above object, the technical solution used in the present invention is: the derivative fast High Performance Liquid Chromatography with Fluorescence Detection of 18 kinds of residual quantity of sulfonamides in beef and mutton.Step comprises:
(1) beef or mutton that do not contain sulfanilamide (SN) material are added in 50mL centrifuge tube as blank sample and testing sample 5g respectively, add 2.5 ~ 8g anhydrous magnesium sulfate, 1 ~ 3g sodium acetate respectively, 1 ~ 10% acetic acid acetonitrile solution (volume ratio) 20mL, PH3 ~ 5, centrifugal 5 ~ the 10min of 10000 ~ 20000r/min high-speed homogenization, 2 ~ 5min, extract 2000 ~ 4000r/min.
(2) supernatant adopts the scavenging material vortex mixed 2 ~ 4min purification and impurity removal added containing multiple adsorbent, 2000 ~ 4000r/min is centrifugal, Aspirate supernatant 10mL blows to be concentrated in 40 ~ 70 DEG C of decompressions or nitrogen and is less than 0.5mL, be settled to 1mL with 10 ~ 20% methanol aqueous solutions, 0.22 μm of miillpore filter must be crossed after shaking up to need testing solution.
(3) chromatographic column that this solution anti-phase key of employing liquid chromatography and C18 are filler is separated, UV-irradiation derives online fast, qualitative according to chromatographic peak retention time, typical curve quantified by external standard method, calculates the residual quantity of 18 kinds of Sulfonamides components in beef and mutton musculature.
Further, sulfa antibiotics of the present invention refers to sulfacetamide (sulfacetamide, SCM), sulphadiazine (sulfadiazine, SDZ), sulphathiazole (sulfathiazole, STZ), sulfapryidine (sulfapyridine, SPD), sulfamethyldiazine (sulfamerazine, SM1), sulfamethazole (sufamoxol, SMX), sulfadimidine (sulfamethazine, SM2), sulfamethoxypyridazine (sulfamethoxypyridazine, SMP), cistosulfa (sulfachloropyridazine, SCP), sulfamethoxazole (sulfamethoxazole, SMZ), Sulfamonomethoxime Sodium (sulfamonomethoxine, SMM), sulfanilamide (SN) Sulfafurazole (sulfisoxazole, SSX), sulfabenzamide (sulfabenzamide, SBZ), sulfaphenazolum (sulfaphenazole, SPP), sulfaclozine sodium (sulfaclozine, SPZ), madribon (sulfadimethoxine, SDM), sulfaquinoxaline (sulfaquinoxaline, SQZ), sulfanitran (sulfanitran, SNT).
Further, the invention is characterized in, in step (1), described extract is 1 ~ 10% acetic acid acetonitrile solution, and its PH is 3 ~ 5, and high-speed homogenization condition is 10000 ~ 20000r/min, centrifugal condition is 2000 ~ 4000r/min, and centrifugal condition is 5 ~ 10min.
Further, the invention is characterized in, in step (2), described purification reagent comprises MgSO
4400 ~ 2000mg, PSA or MCX50 ~ 500mg, C18 or C8 or neutral multi-walled carbon nano-tubes or oh type multi-walled carbon nano-tubes or carboxyl type multi-walled carbon nano-tubes 20 ~ 300mg, phenyl or amino or HLB, Graphon 40 ~ 300mg etc. composition.
Further, the invention is characterized in, in step (3), described anti-phase key and C18 are the chromatographic column of filler is ODSC18 or other liquid-phase chromatographic column being filler with octadecyl bonded silica gel.
Further, the invention is characterized in, the separated flow phase system of described liquid chromatography is for being methanol-water, acetonitrile-water, isopropanol-water, methanol-acetonitrile-water, methanol-isopropanol-water, acetonitrile-isopropanol-water, and in above-mentioned organic phase and aqueous phase all containing or single-phase contain formic acid, acetic acid, phosphoric acid and trifluoroacetic acid, ratio (volume ratio) scope of formic acid, acetic acid, phosphoric acid and trifluoroacetic acid is 0.005 ~ 2%.
Further, the invention is characterized in, the separated flow phase body of described liquid chromatography is degree drip washing such as grade or gradient elution, and the ratio of organic phase is from 1% to 100%.
Further, the invention is characterized in, flow velocity during described liquid-phase chromatographic analysis is 0.5 ~ 1.3mL/min.
Further, the invention is characterized in, the column temperature of described liquid-phase chromatographic column is that room temperature is to 50 DEG C.
Further, the invention is characterized in, described online Post-column photochemical derivatization condition is 2 ~ 12 watts of uviol lamps, wavelength 190nm ~ 400nm, and reactor coil length is 5 ~ 25m, and internal diameter is 0.1mm ~ 0.5mm.
Further, the invention is characterized in, described fluoroscopic examination wavelength is, excitation wavelength is 220 ~ 430nm, and emission wavelength is 401 ~ 520nm.
Further, the invention is characterized in, detecting of this method single sulfonamide is limited to 0.1 ~ 30.0ug/kg, and recovery of standard addition is 60 ~ 120%.
Further, compared with sulfonamides object detecting method in existing meat, the difference of method of the present invention is, apply the improvement QuEChERS being suitable for beef and mutton matrix to extract and purification agent combination, as compared to document " Chen Wanqin; analytical chemistry, 42 volume 573 ~ 578 pages in 2014 " method, significantly shorten the time of sample pre-treatments; 18 kinds of conventional sulfanilamide (SN) compositions detect simultaneously; In addition, the mode that have employed ultraviolet light On-chip derivatization detects, and detection sensitivity improves a lot.
Advantageous Effects of the present invention is: the sample-pretreating method that the present invention adopts, and comprise and extracting and purification, it is easy and simple to handle, consuming time short, completes in 20 ~ 40min; Organic solvent consumption is few, decreases the pollution to environment.
Accompanying drawing explanation
Fig. 1 is 18 kinds of sulfa drugs control sample chromatograms
Fig. 2 is that beef tissue blank adds sulfa drugs sample chromatogram
Fig. 3 is that mutton tissue blank adds sulfa drugs sample chromatogram
1-sulfacetamide; 2-sulphadiazine; 3-sulphathiazole; 4-sulfapryidine; 5-sulfamethyldiazine; 6-5-methoxysulfadiazine; 7-sulfadimidine; 8-sulfamethoxypyridazine; 9-cistosulfa; 10-Sulfamethoxazole; 11-Sulfamonomethoxime Sodium; 12-sulfafurazole; 13-sulfabenzamide; 14-sulfaphenazolum; 15-sulfaclozine sodium; 16-madribon; 17-sulfaquinoxaline; 18-sulfanitran;
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment one
Take homogeneous beef muscle tissue sample 5.00g (being accurate to 0.01g) and add the anhydrous MgSO of 6.00g in advance in 50mL
4, 1.5g sodium acetate polypropylene centrifuge tube in, accurately add 20mL2% acetic acidacetonitrile solution, with homogenizer centrifugal 5min of homogeneous 2min, 4000r/min under 18000r/min, get supernatant to be clean.
Get supernatant 10mL and be placed in 15mL centrifuge tube, in centrifuge tube, add 750mgMgSO in advance
4, 160mgPSA, 100mgGCB and 50mgC
18, by the centrifugal 5min of violent for centrifuge tube vortex mixed 2min, 4000r/min, get supernatant 5mL, blow with nitrogen and be settled to 1mL to nearly dry rear 1mL20% methanol aqueous solution dissolving, cross 0.22 μm of filter membrane, to be determined.
Chromatographic condition
Liquid chromatograph: Waters1525 high performance liquid chromatograph (joining 2475 fluorescence detectors);
Chromatographic column: DikmaPlatisilODSC
i84.6mm × 250mm, filler granularity is 5 μm.
Photochemical derivatization device: uviol lamp power 8w, reactor coil internal diameter 0.25mm, the long 20m of reactor coil.
Column temperature: 36 DEG C.
Flow velocity: 0.7ml/min.
Sample size: 20 μ L.
Determined wavelength: excitation wavelength 320nm, emission wavelength 450nm.
Mobile phase: A0.3% acetic acid aqueous solution, B methyl alcohol, eluent gradient elution requirement is in table 1.
Table 1 eluent gradient elution requirement
| Time (min) | Methyl alcohol | 0.3% acetic acid aqueous solution |
| 0 | 10 | 90 |
| 22 | 35 | 65 |
| 35 | 50 | 50 |
| 40 | 70 | 30 |
| 45 | 10 | 90 |
Linear and detection limit
The range of linearity of table 218 kind of sulfa drugs, regression equation, related coefficient and detection limit
18 kinds of sulfa drugs mark-on recovery test results in table 3 beef sample
Embodiment two
Take homogeneous mutton musculature sample 5.00g (being accurate to 0.01g) and add the anhydrous MgSO of 5.00g in advance in 50mL
4, 2.5g sodium acetate polypropylene centrifuge tube in, accurately add 20mL1.5% acetic acidacetonitrile solution, with homogenizer centrifugal 5min of homogeneous 2min, 4000r/min under 15000r/min, get supernatant to be clean.
Get supernatant 10mL and be placed in 15mL centrifuge tube, in centrifuge tube, add 500mgMgSO in advance
4, the neutral multi-walled carbon nano-tubes of 100mgPSA, 200mgGCB and 50mg, by centrifugal to centrifuge tube vortex mixed 2min, 4000r/min 8min, get supernatant 5mL, blow with nitrogen and be settled to 1mL to nearly dry rear 1mL15% methanol aqueous solution dissolving, cross 0.22 μm of filter membrane, to be determined.
Chromatographic condition
Liquid chromatograph: Waters2965 high performance liquid chromatograph (joining 2475 fluorescence detectors).
Chromatographic column: KromosilODSC
184.6mm × 250mm, filler granularity is 5 μm.
Photochemical derivatization device: uviol lamp power 12w, reactor coil internal diameter 0.25mm, the long 15m of reactor coil.
Column temperature: 35 DEG C.
Flow velocity: 0.7ml/min.
Sample size: 20 μ L.
Determined wavelength: excitation wavelength 320nm, emission wavelength 450nm.
Mobile phase: A0.2% acetic acid aqueous solution, B methyl alcohol, eluent gradient elution requirement is in table 4.
Table 4 eluent gradient elution requirement
| Time (min) | Methyl alcohol | 0.2% acetic acid aqueous solution |
| 0 | 10 | 90 |
| 22 | 35 | 65 |
| 35 | 50 | 50 |
| 40 | 70 | 30 |
| 45 | 10 | 90 |
Linear and detection limit
The range of linearity of table 518 kind of sulfa drugs, regression equation, related coefficient and detection limit
18 kinds of sulfa drugs mark-on recovery test results in table 6 meat samples
Claims (5)
1. the detection method of 18 kinds of residual quantity of sulfonamides in beef and mutton, specific features is to comprise the following steps:
(1) beef of antibiotic-free or mutton are added in 50mL centrifuge tube as blank sample and testing sample 5g respectively, add anhydrous magnesium sulfate 2.5 ~ 8g, sodium acetate 1 ~ 3g respectively, 1 ~ 10% acetic acid acetonitrile solution (volume ratio) 20mL, PH3 ~ 5, centrifugal 5 ~ the 10min of 10000 ~ 20000r/min high-speed homogenization, 2 ~ 5min, extract 2000 ~ 4000r/min;
(2) supernatant adopts the scavenging material vortex mixed 2 ~ 4min purification and impurity removal added containing multiple adsorbent, 2000 ~ 4000r/min is centrifugal, Aspirate supernatant 10mL blows to be concentrated in 40 ~ 70 DEG C of decompressions or nitrogen and is less than 0.5mL, be settled to 1mL with 10 ~ 20% methanol aqueous solutions, 0.22 μm of miillpore filter must be crossed after shaking up to need testing solution;
(3) chromatographic column that this solution anti-phase key of employing liquid chromatography and C18 are filler is separated, ultraviolet light derives online fast, qualitative according to chromatographic peak retention time, typical curve quantified by external standard method, calculates the residual quantity of 18 kinds of Sulfonamides components in beef and mutton musculature.
2. the detection method of 18 kinds of residual quantity of sulfonamides and operation steps thereof in a kind of beef and mutton according to claim 1, is characterized in that: described sulfa antibiotics refers to sulfacetamide (sulfacetamide, SCM), sulphadiazine (sulfadiazine, SDZ), sulphathiazole (sulfathiazole, STZ), sulfapryidine (sulfapyridine, SPD), sulfamethyldiazine (sulfamerazine, SM1), sulfamethazole (sufamoxol, SMX), sulfadimidine (sulfamethazine, SM2), sulfamethoxypyridazine (sulfamethoxypyridazine, SMP), cistosulfa (sulfachloropyridazine, SCP), sulfamethoxazole (sulfamethoxazole, SMZ), Sulfamonomethoxime Sodium (sulfamonomethoxine, SMM), sulfanilamide (SN) Sulfafurazole (sulfisoxazole, SSX), sulfabenzamide (sulfabenzamide, SBZ), sulfaphenazolum (sulfaphenazole, SPP), sulfaclozine sodium (sulfaclozine, SPZ), madribon (sulfadimethoxine, SDM), sulfaquinoxaline (sulfaquinoxaline, SQZ), sulfanitran (sulfanitran, SNT).
3. the detection method of 18 kinds of residual quantity of sulfonamides in a kind of beef and mutton according to claim 1, it is characterized in that, in step (1), the PH of described extract is 3 ~ 5, high-speed homogenization condition is 10000 ~ 20000r/min, centrifugal condition is 2000 ~ 4000r/min, and centrifugal condition is 5 ~ 10min.
4. the detection method of 18 kinds of residual quantity of sulfonamides in a kind of beef and mutton according to claim 1, it is characterized in that, in step (2), described purification reagent comprises MgSO
4400 ~ 2000mg, PSA or MCX50 ~ 500mg, C18 or C8 or neutral multi-walled carbon nano-tubes or oh type multi-walled carbon nano-tubes or carboxyl type multi-walled carbon nano-tubes 20 ~ 300mg, phenyl or amino or HLB, Graphon 40 ~ 300mg etc. composition.
5. the detection method of 18 kinds of residual quantity of sulfonamides in a kind of beef and mutton according to claim 1, it is characterized in that, in step (3), described online post-column derivation condition is 2 ~ 12 watts of uviol lamps, wavelength 190nm ~ 400nm, reactor coil length is 5m ~ 25m, and internal diameter is 0.1mm ~ 0.5mm.
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| CN107576744A (en) * | 2017-09-29 | 2018-01-12 | 沈阳出入境检验检疫局检验检疫综合技术中心 | A kind of method for detecting animal derived food veterinary drug residue |
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