摘要
建立了茶叶中乙撑硫脲残留的柱前衍生-超高效液相色谱-串联四极杆质谱检测方法。样品采用乙腈提取,提取液经QuEChERS基质分散固相萃取净化后采用9-芴基甲基氯甲酸酯(FMOC-CL)柱前衍生;衍生溶液经BEHC18色谱柱(100 mm×2. 0 mm,1. 7μm)分离后进入串联四极杆质谱仪检测,采用同位素内标法定量;流动相为0. 1%(v/v)甲酸-乙腈。该方法对茶叶样品检出限为1. 3μg/kg,定量限为4. 2μg/kg;加标回收率在97. 7%～107. 5%之间,相对标准偏差(RSD,n=6)在2. 1%～10. 0%之间;在1. 0～203. 4μg/L范围内线性回归系数r为0. 999 3。该方法灵敏度高,重现性好,定性定量准确,可有效满足对茶叶中乙撑硫脲残留检测的要求。
A method based on precolumn derivatization along with ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed for the determination of ethylenethiourea residues in tea.The sample was extracted using acetonitrile;the extracting solution was purified by matrix-dispersed solid phase extraction and precolumn derivatization using 9-fluorenylmethyl chloroformate(FMOC-CL).The UPLC separation was carried out on an Acquity BEH C18 column(100 mm×2.1 mm,1.7μm)and quantified using the isotope internal standard method.The mobile phase was 0.1%(v/v)formic acid and acetonitrile.For tea samples,the detection limit of this method was 1.3μg/kg and the limit of quantitation was 4.2μg/kg.The recoveries were in the range 97.7%-107.5%with relative standard deviation(RSD)of 2.1%-10.0%(n=6).The linear correlation coefficient(r)was 0.999 3 over the concentration range 1.0-203.4μg/L.This method showed high sensitivity,good reproducibility,and qualitative and quantitative accuracy,and could be suitable for the detection of ethylenethiourea residues in tea.
作者
郑小严
ZHENG Xiaoyan(Fujian Inspection and Research Institute for Product Quality,Fuzhou 350002,China)
出处
《色谱》
CAS
CSCD
北大核心
2018年第12期1238-1244,共7页
Chinese Journal of Chromatography
