色谱2013，Vol.31Issue(7)：697-702,6.DOI:10.3724/SP.J.1123.2012.12038
加速溶剂萃取-超高效液相色谱-串联质谱快速测定棉花中残留的8种脱叶剂
Determination of eight defoliant residues in cotton by accelerated solvent extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
A novel method has been developed for the rapid extraction and determination of eight defoliants including thidiazuron,butiphos,methabenzthiazuron,abscisic acid,carfentrazone-ethyl,diuron,paraquat,and pyrithiobac-sodium in cotton by accelerated solvent extraction (ASE) coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).The defoliants in cotton were extracted by ASE and the extracts were dried by a rotavapor,then redissolved in the solvents of acetonitrile and water (1 ∶ 9,v/v).The chromatographic analysis was performed on an Acquity UPLC（R） HSS T3 column (50 mm × 2.1 mm,1.8 μm) by a gradient elution employing of acetonitrile and 0.05％ (v/v) formic acid as mobile phases.The analytes were detected by electrospray ionization (ESI) tandem mass spectrometry with multiple reaction monitoring (MRM) in positive ion mode.Good linearities (r ＞ 0.99) were observed between 0.01 and 0.3 mg/L for all the compounds.The recoveries and relative standard deviations (RSDs) were obtained by spiking untreated samples with the eight defoliants at 0.1,0.5 and 1.0 mg/kg.The average recoveries of the eight defoliants were from (84.18 ± 8.04)％ to (95.99 ± 6.76)％.The precision values expressed as RSDs were from 7.04％ to 10.60％ (n =6).The limits of detection were 0.8-29 μg/kg and the limits of quantification were 2.5-96 μg/kg for the analytes.The results showed that the method is simple,rapid,sensitive and accurate,and is suitable for the quantitative determination and confirmation of the eight defoliants in cotton.关键词
加速溶剂萃取/超高效液相色谱-串联质谱/脱叶剂/棉花Key words
accelerated solvent extraction (ASE)/ultra performance liquid chromatographytandem mass spectrometry (UPLC-MS/MS)/defoliants/cotton分类
化学化工引用本文复制引用
吴刚,董锁拽,潘璐璐,赵珊红,王力君,郭方龙,李丹..加速溶剂萃取-超高效液相色谱-串联质谱快速测定棉花中残留的8种脱叶剂[J].色谱,2013,31(7):697-702,6.基金项目
国家公益性项目(201110041) （201110041）
国家质检总局科研项目(2010IK096). （2010IK096）
