TAILIEUCHUNG - HPLC for Food Analysis phần 3

Chuẩn bị mẫu đã được thực hiện theo reference9 250 x mm Spherisorb ODS-2, 5 mm A = sodium acetate đệm, 0,02 M, pH = 4,8 B = ACN / nước (60:40) bắt đầu với B 8% tại 5 phút 8% B tại 7 B 20% min 14 B min 23% tại 16 B tối thiểu 33% tại 19 B tối thiểu 40% ở 21 phút 50% B 26 B 60 phút ở 30 B phút 80% tại 33 B tối thiểu 90% 43 B tối thiểu 90% ở 55 phút 8% B 1,5 ml / phút 20 ml. | Sample preparation Column Mobile phase Gradient Flow rate Injection volume Detector Sample preparation was done according to reference9 250 x mm Spherisorb ODS-2 5 pm A sodium acetate buffer M pH B ACN water 60 40 start with 8 B at 5 min 8 B at 7 min 20 B at 14 min 23 B at 16 min 33 B at 19 min 40 B at 21 min 50 B at 26 min 60 B at 30 min 80 B at 33 min 90 B at 43 min 90 B at 55 min 8 B ml min 20 pl UV-DAD detection wavelengths 275 80 nm 315 80 nm and 360 80 nm reference wavelength 500 100 nm Chromatographic conditions The HPLC method presented here for the analysis of residues of drugs in eggs milk and meat is based on reversed-phase chromatography and multisignal UV-visible diode-array detection UV-DAD . UV spectra were evaluated as an additional identification tool. 10-1 mAU 20- Time min Egg sample Standard HPLC method performance Limit of detection mg kg Repeatability of RT over 10 runs of areas over 10 runs 1 metronidazol 5 2 meticlorpindol 6 3 sulfapyridine 7 4 furazolidone 8 pyrazon ipronidazol chloramphenicol N-acetyl metabolite of 3 9 3-ethopabat 10 benzothiazuron 11 nicarbazin Figure 11 Analysis of residues in an egg sample. Identification through spectra comparison 9. H. Malisch et al. Determination of residues of chemotherapeutic and antiparasitic drugs in food stuffs of anomaly origin with HPLC and UV-Vis diode-array detection J. Liq. Chromatogr. 1988 11 13 . 10. EC Guideline 86 428 EWG 1985. 17 Tetracyclines Tetracyclines are used worldwide as oral or parenteral medication in the form of additives in animal feed. In food-producing animals these drugs exhibit a high degree of activity toward a wide range of 11 Sample preparation Column Mobile phase Gradient Flow rate Column compartment Detector 1 g sample was mixed with citric acid 100 mg . add 1 ml nitric acid 30 or m oxalic acid add 4 ml methanol 5 min in the ultrasonic bath add water up to 10 ml total volume centrifuge inject 100 X 4 mm

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