The long-term use of antibacterial drugs in feeds in large quantities, or their addition in excess of sub-dose levels, can cause residues of antibacterial drugs in animal foods and threaten human health. Therefore, the residues of antibacterial drugs in animal foods have attracted the attention of governments of various countries and various measures have been taken to carry out residue control and testing. The following is a description of macrolide drug multi-residue detection technology in animal foods (including: meat, liver, liver, eggs, milk and honey) as follows:
Japan's Atushii Health Center Mineo used gas chromatography to simultaneously detect 7 penicillins, 3 tetracyclines, 5 aminoglycoside antibiotics, 5 macrolide antibiotics, 2 polyether antibiotics, chloramphenicol and 13 drugs. Thirty-six (36%) of the TCA was used to extract the drug from the meat. The extract was applied to an Amberlite XAD-2 resin column and an activated carbon resin column and then eluted with methanol and 0.01 N HCl-methanol respectively. The eluent was concentrated and dried and then methylated (using pyridine, N, O-bistrimethylsilylacetamide, trimethylsilylimidazole, and trimethylsilyl chloride) using gas chromatography-flame ionization detection. . The method has a recovery rate of 82% for all 36 drugs, and the detection limit for most drugs is equal to that for single drugs.
Delepine et al. of the CNEVA Center of France described a method for the detection of 5 macrolide antibiotics in bovine muscle using the PB/LC/MS method. Gradient elution reverse phase liquid chromatography-MS detection demonstrated the presence of spiramycin, tylosin, tilmicosin, erythromycin, and josamycin residues in bovine muscle. Chloroform was used to extract macrolide antibiotics in the tissues. The extract was purified by solid phase extraction of diols. Five macrolide antibiotics were identified by chemical ionization of anions and cations. The limit of detection for each macrolide antibiotic is 50 μg/kg.
Saitama Prefectural Public Health Association Horie et al. established the simultaneous detection of five macrolides (Josamycin, Leucomycin, Miromicin, Spiramycin and Tellomymycin) in meat by HPLC method. The drug was extracted with 0.3% meta-phosphoric acid methanol (7:3, v/v) and the extract was washed with a Bond Elut SCX (500 mg) cartridge. HPLC separation using a Puresil 5C18 column (150 x 4.6 mm ID), mobile phase 0.025 M phosphate buffer-acetonitrile gradient system (pH 2.5), flow rate 1.0 ml/min. Josamycin, columnar leukemia, Mirosamycin and spiramycin were detected at a wavelength of 232 nm and tyrocin at a detection wavelength of 287 nm. All drugs produced a standard curve with a linear range of 2.5-100 ng. At the 1.0 [mu]g/g addition level, the drug recovery was 70.8-90.4% and the detection limit for each drug was 0.05 [mu]g/g.
The veterinary drug residue Juhel-Gaugain et al. (European Reference Laboratory) has established a method for simultaneous detection of tilmicosin, tylosin, spiramycin, and their major metabolites in the muscles of swine, cattle, and poultry using high-performance liquid chromatography. Acetonitrile was used to extract residual macrolide antibiotics from the muscles. Iso-octane liquid-liquid extraction was used to remove fats. The extracts were purified on Bond Elut C18 cartridges. HPLC separation on an Inertsil ODS3 C18 (150 x 4 mm) column with mobile phase in a 0.05% trifluoroacetic acid-acetonitrile system, tilmicosin-tetracycline and spiramycin-neospiramycin in two modes of shave, Detection wavelengths were 287 and 232 nm, respectively. The test validated the detection performance of pork samples containing 1/2 maximum residue (MRL) to 4 times MRL, and the average recoveries for tilmicosin, tylosin, spiramycin, and neospiramycin were 60. %, 63.5%, 51% and 42%. The limit of detection was 15 μg/kg for tilmicosin and tylosin, 30 μg/kg for spiramycin, and 25 μg/kg for neospiramycin.
University of Barcelona Leal et al. to use liquid chromatography to isolate macrolide antibiotics from animal foods. A high-silica-terminated C18 column was used as the separation column. The mobile phase was a phosphate buffered (pH 2.5)-acetonitrile mixture. Both UV detections were used. System (wavelength, diode array) detection. The limit of detection for spiramycin, tilmicosin, tylosamicin, kitasamicin and josamycin was 6-33 μg/L, and the detection limit for erythromycin and oleandomycin was approximately 400 μg/L. . The test of chicken muscles supplemented with macrolide antibiotics proved that this method is suitable for the simultaneous detection of five macrolide antibiotic residues.
Dubois, CER of Belgium, established the HPLC-MS-MS method for the detection of various tissues (muscle, kidney and liver), 5 macrolides in eggs and milk (Tyracomycin, Tilmicosin, Helicobacter Prime, josamycin, and erythromycin) methods. Roxithromycin was used as an internal standard. The method uses pH 10.5 Tris buffer as an extraction solution, and the sodium tungstate precipitates to remove the protein in the drug extract, and is cleaned on the Oasis solid phase extraction column. The HPLC separation column was a protected column with a Purospher C18 (125 x 3 mm ID) and the mobile phase was a 0.1 M ammonium acetate-acetonitrile gradient system with a flow rate of 0.7 ml/min. In the cation mode, electrospray ionization was performed using the protonated molecule as the parent ion. For each analysis, four product ions were selected for multi-stage reaction monitoring. A negative control and booster sample was analyzed by NRM HPLC-MS-MS for confirmatory studies demonstrating 5 macrolide drug candidates. All sample analyses were demonstrated with four ions, with repeatable ion rates ranging from 2.4-15%. All drugs can be qualitatively and quantitatively tested at a concentration of 1/2 the maximum residue limit. In the European Union recommended concentration range of 0.5 MRL-2 MRL, this method has sufficient specificity, quantification and reproducibility (accuracy: 80-110%, relative standard deviation: 2-13%). This method can extract and analyze 50 samples per day.
Nagata, Chiba Institute of Public Health, Japan used acetonitrile to extract 14 kinds of β-lactam and macrolide antibiotics in bovine muscle. The extract was extracted with n-hexane liquid to remove fat, and TSK-gel was separated by high performance liquid chromatography. ODS-80TM column, acetonitrile-0.05% TCA gradient elution, diode detector quantitative detection. For bovine muscle at a level of 0.1 ppm, the recovery was 63% and the limit of quantitative detection was 0.04 ppm.
The National University of Distance Education of Spain Garcia-Mayor et al. established a rapid, simple and sensitive liquid chromatography UV diode detection for simultaneous determination of seven macrolide antibiotics (erythromycin, oleandomycin, roxithromycin) in goat milk. Residues of penicillin, spiramycin, tylosin and ivermectin). The extraction process of antibiotic residues includes concentrated sodium hydroxide-ethyl acetate treatment of protein-free samples and alkaline hydrolysis to remove fat. The recovery rate for each antibiotic is between 55% and 77% with a relative standard deviation of 1% to 6.5%. Quantitative detection limits: ivermectin 72.4 μg/kg, roxithromycin 48.3 μg/kg, erythromycin, oleandomycin, josamycin, spiramycin, and tylosin 24.1 μg/kg. The method was successfully applied to the detection of multiple drug residues in milk (below the legal maximum concentration level).
Benetti et al. established the simultaneous detection of Lincomycin and 5 macrolide antibiotic residues in honey by liquid chromatography-MS/MS. The analytes were extracted with 0.1 M Tris buffer pH 10.5, purified by solid phase extraction on an OASIS HLB column, and the analytes were chromatographed on a Synergi Hydro-RP reverse phase column using 0.01 M acetate (pH 3.5 Gradient elution with acetonitrile at a flow rate of 0.25 ml/min. According to 2002/657/EC, the linear range, specificity, CCalpha, CCbeta, reproducibility, reproducibility within the laboratory, and recovery rates were validated.
Cultivated Machiner,Agricultural Cultivated Machiner,Farm Cultivated Machiner,Cultivator Rotavator
Shandong Dahua Machinery Co.,Ltd , https://www.agrodahua.com