• Journal of Food Hygiene and Safety
• /
• v.9 no.1
• /
• pp.1-13
• /
• 1994

A Simultaneous determination method was improved for the determination and confirmation of zeranol, zearalenone, as well as their isomers and metabolites, in beef. The analytes were extracted from tissue by CH3CN, hydrolyzed enzymatically(for glucuronide conjugates), cleaned up by a strong basic anion exchange resin combined with a liquid/liquid partitioning, derivatized using MSTFA and confirmed, quantified by GC/MS/SIM with a internal standard, zearalane. The results were as follows : (1) all the estrogens were separated on the GC/MS chromatogram under the extraction method and the chromatographic conditions improved, the retention times of zearalane-TMS2, zearalanone-TMS2, zearalenone-TMS2, zeranol-TMS3, taleranol-TMS3, and $\alpha$-zearalenol-TMS3, $\beta$-zearalenol-TMS3, were 18.49, 19.44, 19.63, 19.71, 19.79 and 19.99, 20.08 minutes, respectively. (2) The calibration curves of residual zeranol, zearalenone and their metabolites showed constantly linear(r=0.99) in the range of 5~20 ng. The minimum detection concentration of residual zeranol, zearalenone and their metabolites was 1 ppb. (3) The total average recovery of residual zeranol, zearalenone and their metabolites from spiked beef was 60.2%(CV=29.7%) at the 1 ppb and 63.5%(CV=26.5) at the 2 ppb, 72.9%(CV=18.2%) at the 4 ppb. (4) The preservation method for 6 estrogens was improved for the fast running time(21 min) and MSTFA was utilized for derivatizing 6 estrogens for improvement of recovery, for good resolution, for characteristic mass spectra unlike Jose's method and Tina's method. The utilization of zearalane as internal standard showed good quantification result for zeranol, zearalenone, as well as their isomers and metabolites, in beef.

• Analytical Science and Technology
• /
• v.21 no.6
• /
• pp.526-534
• /
• 2008

To determine the trace level of synthetic and natural hormones in food, the improvement of official analytical method and new development of simultaneous determination of hormones were established. On the basis of developed analytical method, the background level of natural hormones and distribution of residual hormones were monitored in meat. Target hormones were six natural hormones such as estrogens ($17{\beta}$-estradiol, $17{\alpha}$-estradiol, estrone), androgens ($17{\beta}$-testosterone, $17{\alpha}$-testosterone), and gestagens (progesterone) and three synthetic hormones such as DES, zeranol, and taleranol. These hormones were analyzed by gas chromatographymass spectrometry. Newly developed multi-residue analysis method was applied for meat sample which were collected from market in the capital region and monitored the presence of residues of synthetic and natural steroid hormones. No residue of synthetic hormones were detected and endogenous level of progesterone was detected in cattle, pig and liver samples tested.