A liquid chromatographic method, using matrix solid-phase dispersion (MSPD) is developed for the extraction of residual furazolidone in chicken eggs. Blank or fortified egg samples (0.5 g) were blended with Octadecylsilyl (Bulk C,,, 40 pm, 18%. load, endcapped. 2 g) derivatized silica. After homogenization, C,,/egg and Na2S0, matrix were transferred to a column made of 10 ml glass synnge and filter paper and compressed 4.0-4.5 ml volume. The column was washed with 8 ml of hexane and dried under N, gas. Furazolidone was eluted with acetonitrile (8 ml) under gravity. The eluate containing furazolidone was free from interfering compounds when analyzed by HPLC with UV detection (365 nm, photodiode array). Calibration curves were linear (r = 0.99985) and inter- (1.47%) and intra-assay (5.29%) variabilities for the concentration range examined (7.8-497 ngig of eggs, 20 pl injection volume) were indicative of an acceptable methodology for the analysis of furazolidone. Average recovery of furazolidone added to egg was 96.2%. The limit of detection for the proposed method was 1 ng/g for furazolidone. The method using MSPD is proposed as an alternative assay to the classical method which involves the use of large volumes of a harmful solvent and requires a long tedious separation and clean-up processes prior to its determination.
This study was conducted to evaluate the MSPD and HPLC method about simultaneous determination for residual synthetic antimicrobials of sixteen species such as sulfonamide etc. in livestock products. Elution solvent used in HPLC was ethylacetate : acetonitrile (4 :1), and mobile phases for solvent A and B were water : methanol : acetonit rile : phosphric acid (700:250:50:0.2) and 100% acetonitrile respectively. The detector and absorbency used in HPLC was UV 266 nm. This study showed the reduction effect of 99.1% for organic solvents, 94% for experimental steps, 95% for analytical time and manpower and 98.9% for costs compared with korea food standard method. The average recovery rates for chicken, bovine, pork and milk were 67.7% 96.2 %, 67.7%-96.6%, 70.0%-96.2%, and 13.8%-97.8%.
A simple, rapid and simultaneous analytical method is described for the detection of Sulfonamide and Tetracycline residues, i.e., Sulfamerazine (SMR), Sulfamethazine (SMT), Sulfamonomethoxine (SMM), Sulfadimethoxine (SDM), Sulfaquinoxaline (SQN), Oxytetracycline (OXY), Tetracycline (TC), Chlortetracycline (CTC). Blank control and sulfonamide and tetracycline fortified fish muscle samples (0.5 g) were blended with octadecylsilyl (C,e, 40 gm, 21% load, 60Å) derivatized silica packing material (2 g). Blended fish samples were washed with hexane, then, benzene and dichloromethane were used for the elution of tetracycline and sulfonamide, respectively, The eluants containg tetracycline and sulfonamide were analyzed by HPLC. Correlation coefficients of standard curves for individual sulfonamide and tetracycline isolated from fortified samples were linear (0.9993±0.0003-0.9997±0.0003, 0.9493±0.078-0.9753±0.036), respectively, The average percentage recoveries of sulfonamide and tetracycline ranged as 80.86-96.52% to 85.88-92.23%, and 30.01-37.12% to 65.89-73.40%, for the concentration range (0.1--1.0 ppm) examined, respectively. Limit of detection for sulfonamide was 0. 05 ug/g, then, tetracycline was 0.1 ug/g. Detection of quantitation of sulfonamide residue was 0.0012 ppm for SMR in Paralichthys Odiuacleus and 0.0020 ppm for SMR, 0.015 ppm for SMM in Cyprinus Carpio. The applicability of this procedure is demonstrated by separation and detection of incurred tetracycline and sulfonamide residues in fish muscle tissue.