Fathy Mehaya | National Research Centre (original) (raw)

Papers by Fathy Mehaya

High-performance liquid chromatographic method with diode-array detection (HPLC-DAD) was optimise... more High-performance liquid chromatographic method with diode-array detection (HPLC-DAD) was optimised and validated for determination of tetracyclines (TCs) residue in chicken meat and liver through evaluating each step of various methods. The principle steps involved ultrasonic-assisted extraction of TCs from chicken samples by 2 ml of 20% trichloroacetic acid and citrate buffer (pH 4) which gave a clearer supernatant and high recovery, followed by centrifugation and purification on SPE (Strata C18-E cartridge) using 10 ml of 0.01 M methanolic oxalic acid for TCs elution. Separation was on reversedphase column (Nuclosil 100 C18, 25 cm  4.6 mm ID, 5 l) by multisteps gradient elution which provided a better chromatographic peak resolution and the late eluting peaks were as sharp as those eluting earlier. Monitoring was at 351 nm which gave a higher detector response factor. Validity study of the method revealed that all obtained calibration curves showed good linearity (r 2 > 0.999) over the range of 50-5000 ng. Sensitivity was found to be 1.44, 1.90, 0.95 and 1.23 ng for OTC, TC, CTC and DC, respectively. Accuracy was in the range of 71. 88-92.44.3% and 68.88-84.84% for meat and liver, respectively. Precision was lower than 10% in all cases indicating that the method can be used as a validated method. Limit of detection (LOD) was found to be 4.4, 5, 13 and 10 ng for OTC, TC, CTC and DC, respectively. The corresponding values of limit of quantitation (LOQ) were 10, 13, 27 and 22 ng.

The incidence of tetracyclines' (TCs) residue (oxytetracycline, tetracycline, chlorotetracycline ... more The incidence of tetracyclines' (TCs) residue (oxytetracycline, tetracycline, chlorotetracycline and doxycycline) in fresh chicken samples (meat and liver) collected during one year was recorded. TC residues were analysed using an HPLC-DAD method. The limit of detection for meat was 4.4, 5, 10 and 7 ng g À1 for OTC, TTC, CTC and DOC, respectively, compared with 5.5, 6, 12 and 9 ng g À1 stated for liver. The recovery of the method ranged from 91% to 70% depending upon both matrix type and tetracycline kind. The results revealed that 66 (44%) samples contained TC residues including 21 (42%) breast, 19 (38%) thigh and 26 (52%) liver samples. The corresponding contaminated ranges were 124-5812, 107-6010 and 103-8148 mg kg À1 . A total of 12 (8%), 13 (7.33%) and 20 (13.33%) samples of breast, thigh and liver, respectively, had TC residues above the Codex maximum residue limit (MRL). Liver samples had a higher incidence and level than those found in breast or thigh samples.

High-performance liquid chromatographic method with diode-array detection (HPLC-DAD) was optimise... more High-performance liquid chromatographic method with diode-array detection (HPLC-DAD) was optimised and validated for determination of tetracyclines (TCs) residue in chicken meat and liver through evaluating each step of various methods. The principle steps involved ultrasonic-assisted extraction of TCs from chicken samples by 2 ml of 20% trichloroacetic acid and citrate buffer (pH 4) which gave a clearer supernatant and high recovery, followed by centrifugation and purification on SPE (Strata C18-E cartridge) using 10 ml of 0.01 M methanolic oxalic acid for TCs elution. Separation was on reversedphase column (Nuclosil 100 C18, 25 cm  4.6 mm ID, 5 l) by multisteps gradient elution which provided a better chromatographic peak resolution and the late eluting peaks were as sharp as those eluting earlier. Monitoring was at 351 nm which gave a higher detector response factor. Validity study of the method revealed that all obtained calibration curves showed good linearity (r 2 > 0.999) over the range of 50-5000 ng. Sensitivity was found to be 1.44, 1.90, 0.95 and 1.23 ng for OTC, TC, CTC and DC, respectively. Accuracy was in the range of 71. 88-92.44.3% and 68.88-84.84% for meat and liver, respectively. Precision was lower than 10% in all cases indicating that the method can be used as a validated method. Limit of detection (LOD) was found to be 4.4, 5, 13 and 10 ng for OTC, TC, CTC and DC, respectively. The corresponding values of limit of quantitation (LOQ) were 10, 13, 27 and 22 ng.

The incidence of tetracyclines' (TCs) residue (oxytetracycline, tetracycline, chlorotetracycline ... more The incidence of tetracyclines' (TCs) residue (oxytetracycline, tetracycline, chlorotetracycline and doxycycline) in fresh chicken samples (meat and liver) collected during one year was recorded. TC residues were analysed using an HPLC-DAD method. The limit of detection for meat was 4.4, 5, 10 and 7 ng g À1 for OTC, TTC, CTC and DOC, respectively, compared with 5.5, 6, 12 and 9 ng g À1 stated for liver. The recovery of the method ranged from 91% to 70% depending upon both matrix type and tetracycline kind. The results revealed that 66 (44%) samples contained TC residues including 21 (42%) breast, 19 (38%) thigh and 26 (52%) liver samples. The corresponding contaminated ranges were 124-5812, 107-6010 and 103-8148 mg kg À1 . A total of 12 (8%), 13 (7.33%) and 20 (13.33%) samples of breast, thigh and liver, respectively, had TC residues above the Codex maximum residue limit (MRL). Liver samples had a higher incidence and level than those found in breast or thigh samples.