Ali M S, Sun T, McLeroy G E, Phillippo E T
U.S. Department of Agriculture, Food Safety and Inspection Service, Atlanta, GA 30604, USA.
J AOAC Int. 2000 Jan-Feb;83(1):39-52.
A liquid chromatographic (LC) multiresidue screening procedure was developed for determination of eprinomectin, moxidectin, abamectin, doramectin, and ivermectin in beef liver at 0, 25, 50, and 100 ppb levels. A procedure using low resolution LC/atmospheric pressure chemical ionization (APCI) mass spectrometry (MS) was developed with further purification steps added to the quantitative LC method to confirm residues. Acetonitrile extracts of liver, prior to derivatization for LC analysis, were further purified by using a C8 solid-phase extraction cartridge and an alumina-B cartridge. The purified extract was analyzed by injection into an LC/positive ion APCI MS. Identity of the compound was confirmed by comparison of its retention time and relative intensity data with those of a standard or recovery from a fortified control liver sample. Anthelmintic drugs in acetonitrile extracts of liver containing eprinomectin, moxidectin, abamectin, doramectin, and ivermectin at 25 ppb, the lowest level of fortification used in the LC determinative method, were successfully confirmed.
开发了一种液相色谱(LC)多残留筛查程序,用于测定牛肝中0、25、50和100 ppb水平的埃普利诺菌素、莫西菌素、阿维菌素、多拉菌素和伊维菌素。开发了一种使用低分辨率LC/大气压化学电离(APCI)质谱(MS)的程序,并在定量LC方法中增加了进一步的纯化步骤以确认残留。肝脏的乙腈提取物在进行LC分析衍生化之前,通过使用C8固相萃取柱和氧化铝-B柱进一步纯化。将纯化后的提取物注入LC/正离子APCI MS中进行分析。通过将其保留时间和相对强度数据与标准品的数据进行比较,或与加标对照肝脏样品的回收率进行比较,来确认化合物的身份。成功确认了牛肝乙腈提取物中含有25 ppb(LC测定方法中使用的最低加标水平)的埃普利诺菌素、莫西菌素、阿维菌素、多拉菌素和伊维菌素的驱虫药物。