A large supplier of KFC and McDonald's was exploded at the end of November 2012. A chicken raised from hatching to serving on the table only took 45 days and was fed with feed and medicine. CCTV also exposed many places in Shandong In chicken farms, white chickens were fed antibiotics or antiviral drugs. In some places, chickens were even given amantadine, ribavirin, and dexamethasone, which were banned by the state, and antibiotics such as chloramphenicol and furans were detected. Substances have hidden safety risks to human health.

The detection methods of illegal drugs such as antibiotics and hormones involved in this incident are:

1. GBT 20741-2006 Determination of dexamethasone residues in livestock and poultry meat by liquid chromatography-tandem mass spectrometry

2. GBT 20752-2006 Determination of nitrofuran metabolite residues in pork, beef, chicken, pork liver and aquatic products liquid chromatography-tandem mass spectrometry

3. Announcement No. 781 of the Ministry of Agriculture -2-2006 Determination of chloramphenicol residues in foods of animal origin High performance liquid chromatography-tandem mass spectrometry

4. Announcement No. 958 of the Ministry of Agriculture -6-2007 Determination of Dexamethasone Residue in Pig Edible Tissue High Performance Liquid Chromatography

5. Ministry of Agriculture Announcement No. 1025-12-2008 Detection of tetracycline residues in chicken and pork by liquid chromatography-tandem mass spectrometry

6. Ministry of Agriculture Announcement 781-4-2006 Determination of nitrofuran metabolite residues in foods of animal origin High performance liquid chromatography-tandem mass spectrometry

7. DB32 / T 1165-2007 Determination of the total residues of ribavirin and its metabolites in chicken liver Liquid chromatography-tandem mass spectrometry

8. DB32 / T 1163-2007 Determination of amantadine residue in chicken liver Liquid chromatography-tandem mass spectrometry

The above standard methods use solid phase extraction to pre-purify the sample. The FREESTEYLE SPE of German LCTech company completely matches the solid phase extraction process of the standard method that is activation, loading, cleaning, drying and eluting. Combined with EVA, the solid phase extraction eluent is concentrated online to a specified volume, fully realizing the automation of sample preparation and processing samples around the clock, greatly improving the efficiency and efficiency of the laboratory.

The following are the test results of samples processed by solid phase extraction, for reference only!

Detection of tetracycline residues in chicken and pork

Solid phase extraction column online concentration method:

Solid phase extraction column: HLB column (60mg / 3ml)

1. Activation: 5ml methanol and 5ml water, speed 1ml / min

2. Sample loading: 8ml sample extraction solution is passed through the column, the speed is 0.5 ~ 1ml / min

3. Cleaning: 5ml water, then 5ml 5% methanol aqueous solution, speed 1ml / min

4. Drying: air or nitrogen blow drying

5. Elution: 5ml methanol elution, speed 0.5ml / min

6. Online concentration conditions: nitrogen blow dry or concentrate to dry, temperature 40 ℃

7. Make up to volume with methanol + water (3: 7) to 1ml, transfer to 1ml sample bottle and analyze by LC-MS

Nitrofurans in pork, beef, chicken, liver and aquatic products

Determination of metabolite residues

Solid phase extraction column online concentration method:

Solid phase extraction column: HLB column (60mg / 3ml)

1. Activation: 5ml methanol and 10ml water, speed 1ml / min

2. Sample loading: the supernatant passes through the column at a speed of 2ml / min

3. Cleaning: 10ml water cleaning, speed 1ml / min

4. Drying: air or nitrogen blow drying

5. Elution: 5ml ethyl acetate, the speed is 0.5ml / min

6. Online concentration conditions: nitrogen blow dry or concentrate to dry, temperature 40 ℃

7. Make up to 1ml with sample constant volume solvent, transfer to 1ml sample bottle and analyze by LC-MS

Determination of dexamethasone residues in livestock and poultry meat

Solid phase extraction column online concentration method:

Solid phase extraction column: BOND-ELUT Si column (500mg / 3ml)

1. Activation: 2ml acetone: n-hexane = 2: 8, speed 1ml / min

2. Sample loading: The extraction solution passes through the column at a speed of 1 ~ 2ml / min

3. Drying: air or nitrogen blow drying

4. Elution: 6ml acetone: n-hexane = 4: 6, speed 1 ~ 3ml / min

5. Online concentration conditions: nitrogen blow drying or concentration to dryness, temperature 40 ℃

6. Make up to 1ml with mobile phase, transfer to 1ml sample vial and analyze by LC-MS

Determination of amantadine residues in chicken liver by liquid chromatography-tandem mass spectrometry

Solid phase extraction column online concentration method:

Solid phase extraction column: Oasis MCX column (60mg / 3ml)

1. Activation: 3ml methanol and 3ml water, speed 1ml / min

2. Sample loading: 5ml of extraction solution passes through the column at a speed of 1ml / min

3. Cleaning: Use 3ml of 2% hydrochloric acid and 3ml of methanol in turn, at a speed of 1ml / min

4. Elution: 5ml ammonia-methanol-isopropanol solution (5:80:15), the speed is 0.5ml / min

5. Online concentration conditions: nitrogen blow dry or concentrate to dry, temperature 50 ℃

6. Make up to 1ml with methanol-water-formic acid (10: 90: 0.1) solvent, transfer to 1ml sample bottle and analyze by LC-MS

Chromatogram of chicken blank matrix and amantadine added to chicken

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