Reuvers T, Perogordo E, Jiménez R
Servicio de Bromatología, Centro nacional de Alimentación, majadahonda, Spain.
J Chromatogr. 1991 Apr 5;564(2):477-84. doi: 10.1016/0378-4347(91)80516-f.
A rapid and sensitive screening method for the determination of residues of diethylstilbestrol in edible animal tissue is described. The analyte was extracted from the tissue with tert.-butyl methyl ether, reextracted with 1 M sodium hydroxide and further cleaned up by solid-phase extraction with C18 cartridges. Analysis was performed by isocratic elution with a phosphate-buffered mobile phase, methanol-0.05 M phosphate buffer pH 3.5 (67:33), on a Nucleosil 5-microns C18 column with electrochemical detection at +0.90 V. The average recovery of trans-diethylstilbestrol in spiked samples is 66%, with a standard deviation of 14% (n = 22) in the range 0.5-2.0 microgram/kg. The detection limit is 0.1-0.2 microgram/kg, although at this level other compounds may interfere and give rise to false positive results.
本文描述了一种快速、灵敏的检测食用动物组织中己烯雌酚残留量的筛查方法。分析物用叔丁基甲醚从组织中提取，再用1M氢氧化钠反萃取，并通过C18柱固相萃取进一步净化。采用磷酸盐缓冲流动相（甲醇-0.05M磷酸盐缓冲液pH 3.5，67:33）进行等度洗脱，在Nucleosil 5微米C18柱上，于+0.90V进行电化学检测。加标样品中反式己烯雌酚的平均回收率为66%，在0.5 - 2.0微克/千克范围内，标准偏差为14%（n = 22）。检测限为0.1 - 0.2微克/千克，不过在此水平下其他化合物可能会产生干扰并导致假阳性结果。
