Zeranol (Z) is an estrogenic growth-promoting agent synthesized from mycotoxin zearalenone (Zen). Inadvertent consumption of Z and its structural analogs from meat or grain products remain a food safety concern. An ec...Zeranol (Z) is an estrogenic growth-promoting agent synthesized from mycotoxin zearalenone (Zen). Inadvertent consumption of Z and its structural analogs from meat or grain products remain a food safety concern. An economic and rapid high performance liquid chromatography method with electrochemical detection using disposable screen-printed carbon electrode is developed for determination of Z, Zen and 3 major metabolic analogs α-zearalenol (α-Ze), β-zearalenol (β-Ze), and β-zearalanol (β-Za). The electrochemical method was validated for application in food matrices including beef, pork, feed and cereal after optimized liquid and/or solid-phase extraction procedures. All 5 Z analogs were separated in 10 minutes with the limits of detection ranging from 15 ng/ml for α-Ze and 25 ng/ml for Z and Zen;the limit of quantitation ranged from 40 50 ng/ml. The recoveries were all above 75% regardless of matrix types and extraction procedures. The intra and inter day variations were both less than 6% at the nominal concentration of 1 μg/ml and less than 13% at 100 ng/ml level. Chromatographically time-matched peaks of Z, α-Ze and β-Za were observed in moldy feed, cereal and rice with high productivity, indicating possible grain-specific Zs exposure for animals and human. Proper exercise of preservative procedures for grain and grain products to prevent it from mold production is imperative. The simplicity and reproducibility of this method affords quick and reliable quantitation of multiple types of Z analogs in food products and can offer semi-confirmative information comparable to UV detection and supplementary to ELISA screening.展开更多
文摘Zeranol (Z) is an estrogenic growth-promoting agent synthesized from mycotoxin zearalenone (Zen). Inadvertent consumption of Z and its structural analogs from meat or grain products remain a food safety concern. An economic and rapid high performance liquid chromatography method with electrochemical detection using disposable screen-printed carbon electrode is developed for determination of Z, Zen and 3 major metabolic analogs α-zearalenol (α-Ze), β-zearalenol (β-Ze), and β-zearalanol (β-Za). The electrochemical method was validated for application in food matrices including beef, pork, feed and cereal after optimized liquid and/or solid-phase extraction procedures. All 5 Z analogs were separated in 10 minutes with the limits of detection ranging from 15 ng/ml for α-Ze and 25 ng/ml for Z and Zen;the limit of quantitation ranged from 40 50 ng/ml. The recoveries were all above 75% regardless of matrix types and extraction procedures. The intra and inter day variations were both less than 6% at the nominal concentration of 1 μg/ml and less than 13% at 100 ng/ml level. Chromatographically time-matched peaks of Z, α-Ze and β-Za were observed in moldy feed, cereal and rice with high productivity, indicating possible grain-specific Zs exposure for animals and human. Proper exercise of preservative procedures for grain and grain products to prevent it from mold production is imperative. The simplicity and reproducibility of this method affords quick and reliable quantitation of multiple types of Z analogs in food products and can offer semi-confirmative information comparable to UV detection and supplementary to ELISA screening.
基金Project supported by the National Natural Science Foundation of China (No. 30471155) the Agriculture Key Technologies R & D Program of Shanghai (No. (2003) 9-4), China
文摘建立了动物源性食品中6种玉米赤霉醇类化合物和氯霉素残留量的复合免疫亲和柱净化、液相色谱-串联质谱（LC-MS / MS）分析方法。样品（鱼肉、肝脏、牛奶、蜂蜜）经β-葡萄糖苷酸/硫酯酸复合酶酶解后用乙醚提取，提取液经氮气吹干，残渣用50％乙腈溶液复溶后过滤，滤液用 PBS 溶液稀释，经复合免疫亲和柱富集净化后供 LC-MS /MS 检测，采用多反应监测（MRM）模式进行定量和定性分析，外标法定量。结果表明，7种目标物的检出限（ S / N ＝3）在0.04~0.10μg / kg 之间，线性相关系数（R2）≥0.9990，平均回收率为70.9％~95.6％，相对标准偏差为2.0％~11.8％。该方法灵敏度高、重现性好，适用于动物源性食品中痕量玉米赤霉醇类药物和氯霉素残留的测定。
