This standard specifies the detection method for oxytetracycline, tetracycline and chlortetracycline residues in livestock and poultry meat. This standard is applicable to the determination of oxytetracycline, tetracycline and chlortetracycline residues in various livestock and poultry meat. The detection limit of this standard is 0.15mg/kg for oxytetracycline, 0.20mg/kg for tetracycline and 0.65mg/kg for chlortetracycline. GB/T 5009.116-2003 Determination of oxytetracycline, tetracycline and chlortetracycline residues in livestock and poultry meat (HPLC method) GB/T5009.116-2003 Standard download decompression password: www.bzxz.net

IS 57.040
National Standard of the People's Republic of China
GB/T5009.116—2003
Replaces GB/T14931.1-:994
Determination of oxytetracyline, etracyline and chlortetracyline residues in livestock and poultry meat (HPLC method) (HPC) Issued on August 11, 2003
Ministry of Health of the People's Republic of China
China National Standardization Administration
Implementation on January 1, 2004
GB/T5009.116—2003
This standard replaces GB/T14931.1—:994, Determination of ten-proof rate, four-negative factors and gold content in real meat (HPLC chromatography). t||Compared with GB/T4931,1·-1994, the main revisions of this standard are as follows: The Chinese name of the standard was revised to the Chinese name of the standard, the Chinese name of the standard was changed ... FK
1 Scope
Animal, meat, sergeant, tetracycline capsule, chlortetracycline residue determination (high performance liquid chromatography method) The standard stipulates the determination of chlortetracycline residues in China, tetracycline, gold science and technology, this standard applies to various high-strength chlortetracycline, tetracycline, gold science and technology, and micro-tasting, (A/T 5009.116—2003
The detection limit of this standard is 0.15rR/kg of tetracycline, a.2mgkg of chloramine, and 0.65ng/kg of chloramine. 2. The original sample is extracted, and the sample is connected to the microporous membrane, separated by phase chromatography, and detected by an external exchanger. The peak sequence is chloramine, tetracycline, and chloramine, and the standard addition method is correct. 3.1 Ethylene (analyte)
3.2U, 1mol/L phosphorus dioxygen material falls into the liquid grid and collects 1.53gt box to confirm -0.0 1g>Sodium dihydrogen phosphate (NsI, PH, 2IE())>Dry distilled water, make up to 10)mL, pass through a sensitive porous membrane (0.45um), prepare 3.3 above-mentioned powder (QT) standard limit: weigh 0.01Ug of soil and be accurate to ±3.00018). Dissolve it in U.1mol/l alcohol solution and determine it in 10.00ml. This solution contains 7g of tetracycline per liter. 3.4 Tetracycline TC>Standard minus: take 0.0010g of tetracycline and be accurate to ±0M1). Decompose it with 0.1mol/l hydrochloric acid solution and determine it in 10.00mL. This solution contains 1g of tetracycline per milliliter. 3. Gold standard solution: weigh 0.0200 (accuracy: 0.0001). Dilute to 10.0mL with distilled water. Each liter contains 1mg of gold. The main standard is converted at 1% unit/%. 3.3~3.5% is added to 4% and stored. It can be stored for 1 week. 3. Preparation: Take 3.3.3.1 standard solution, 2.0ml of iridium, 3.5ml of standard solution, and add to a 1mM volumetric bottle. Add water to the scale. This solution contains 0.1ng of iridium, 0.1ng of tetracycline, 0.2ng of dapoxetine per liter. Prepare it before use with 3.75% perchloric acid solution and 4% tantalum. t||High efficiency phase-to-phase tower instrument (ITFT.E): UV detector 5 Chromatographic conditionsbzxz.net
5. Gui, ODS-C (5Jh2mmX1scm.
5.2 Detection wavelength: 355,
5.3 Hot amount 112AUFS
5.4 Mixing: room temperature adjustment-
5.5: 1.0mL/min
5.6 Inlet: 10L.
5.7 Mobile phase t 0.0mol/l trichloroethylene solution (adjust the pH value of the solution to 2.5 with 30 times nitric acid) = 5-station, use ultrasonic to remove the gas for 1nmin.
GB/T 5009.1162003
6 Analysis steps
6.1 Sample determination: Weigh 5.00g (±0.01g) of chopped sugar sample (51nm), weigh at 50mJ, add 25.0mL of 5% hydrofluoric acid into a conical flask, extract 10trin on a vibrating decanter, pour into a centrifuge tube, centrifuge at 2000r/min for 3min, take the supernatant, filter through n.45\: membrane, take 1uL for injection, record the peak height, and check the content from the working curve. 6.2 Working curve: Weigh 7 portions of chopped meat samples, 5.00g each (sugar content to ±0.01g), add mixed standard 0, 25.50.100.150260, 2502L (containing ±0.1% tetracycline, 2.3, 5.0, 10 ..15.4,20,0,85μg>；U,5.C,10.V20.0.30.0.40.0.59.0g), according to the method of 6.1, the peak height is the numerical coordinate, and the antibiotic content is the horizontal coordinate to draw the working curve.
6.3 Conclusion and calculation
Calculate according to the following formula:
4×1000
mx1(100
Where:
The antibiotic content in the sample, the unit is milligram per kilogram (m/kg): 4——The antibiotic mass measured in the test box, the unit is gram (\g) or the selected unit is gram (),
7 Precision
The running difference between two independent determinations obtained under repeatability shall not exceed 1% of the arithmetic mean value.au
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