Ye Lin
U.S. Food and Drug Administration, Southeast Regional Laboratory, 60 8th Street NE, Atlanta, GA 30309, USA.
Food Chem. 2017 Aug 1;228:70-76. doi: 10.1016/j.foodchem.2017.01.139. Epub 2017 Feb 1.
A simple, rapid, selective and sensitive LC-MS/MS method was developed and validated for the determination of isoeugenol in finfish using an off-line dansylation derivatization step to enhance signal intensity. The sample was extracted with 10mL acetone using a tissue homogenizer, followed by derivatization with dansyl chloride and analysis by liquid chromatography tandem mass spectrometry. The method detection limit ranged from 0.2 to 0.7ngg in six fish species. The limit of quantification was 2.5ngg in each species. Recoveries of isoeugenol at three different levels (5, 10 and 20ngg) over two different days ranged from 91.2% to 108.0%. Precision (%RSD) values determined at 10ngg were 4.3%, 8.0%, 5.3%, 5.1%, 2.6% and 8.0% for tilapia, catfish, trout, salmon, hybrid striped bass and yellow perch, respectively. Studies of linearity in the range 2.5-40ngg produced determination coefficients (R) above 0.997 for all matrices.
建立并验证了一种简单、快速、选择性好且灵敏的液相色谱-串联质谱法，用于测定鱼类中的异丁香酚，该方法采用离线丹磺酰化衍生步骤来增强信号强度。使用组织匀浆器将样品用10mL丙酮提取，随后用丹磺酰氯进行衍生化，并通过液相色谱串联质谱法进行分析。该方法在六种鱼类中的检测限为0.2至0.7ng/g。每种鱼类的定量限为2.5ng/g。在两天内，异丁香酚在三个不同水平（5、10和20ng/g）的回收率为91.2%至108.0%。在10ng/g水平下测定的罗非鱼、鲶鱼、鳟鱼、三文鱼、杂交条纹鲈和黄鲈的精密度（%RSD）值分别为4.3%、8.0%、5.3%、5.1%、2.6%和8.0%。在2.5 - 40ng/g范围内的线性研究表明，所有基质的测定系数（R）均高于0.997。
