摘要
建立了动物肌肉组织中己烯雌酚残留的液相色谱-串联质谱分析方法。样品用乙腈-甲酸溶液均质提取，以乙腈-水（体积比85：15）为流动相经反相色谱柱分离后，采用多反应监测（MRM）负离子模式检测，定性离子对为m／z266．9／237．0和266．9／251．0；其中m／z266．9／251．0用于外标法定量。空白样品及其加标实验结果表明，特征离子相对强度比值稳定，无基质干扰，结合保留时间可实现准确的定性定量，方法检出限为0．10μg／kg（S／N=3），不同肌肉基质样本添加水平在0．5～5．0μg／kg时，平均回收率为82％～96％，相对标准偏差（n=6）为3．7％-6．4％。
An analytical method for the determination of diethylstilbestrol （DES） residues in animal muscles with HPLC -MS/MS was established. The sample was homogenized and extracted with aceto- nitrile -formic acid solution. Following reverse phase HPLC separation with CHsCN -H20 （85 ： 15 by volume）, the extractant was determined by tandem mass spectrometry, in the negative electrospray ion- ization mode with multiple reaction monitoring of two precursor-product ion pairs： m/z 266. 9→237.0 and 266. 9→251. 0. The transition of m/z 266. 9→251.0 was also used for quantitation. Analysis of blank and fortified samples showed that the relative intensity of the DES identification ion pairs in various matrices was stable. And there was no matrix interference with these confirmatory transitions. Combining with retention time, the method could be used for accurate qualitative analysis. The LOD （ S/N = 3 ） was 0. 10 μg/kg. At the spiking levels of 0. 5 - 5.0 μg/kg for various muscle matrices, the average recoveries were 82% -96% with RSD（ n = 6） values between 3.7% and 6.4% .
出处
《分析测试学报》
CAS
CSCD
北大核心
2007年第6期823-826,共4页
Journal of Instrumental Analysis
