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

作　　者：吴刚 董锁拽 潘璐璐 赵珊红 王力君 郭方龙 李丹 

机构地区：[1]浙江省检验检疫科学技术研究院,浙江杭州310015 [2]浙江出入境检验检疫局丝类检测中心,浙江杭州310012 [3]浙江立德产品技术有限公司,浙江杭州310015

出　　处：《色谱》2013年第7期697-702,共6页Chinese Journal of Chromatography

基　　金：国家公益性项目(201110041);国家质检总局科研项目(2010IK096)

摘　　要：采用加速溶剂萃取结合超高效液相色谱-串联质谱(UPLC-MS/MS)技术,建立了一种快速提取和测定棉花中8种脱叶剂(噻苯隆、脱叶磷、甲基苯噻隆、脱落酸、氟酮唑草酯、敌草隆、百草枯、嘧草硫醚)的分析方法。样品经提取、浓缩,乙腈-水溶液(1∶9,v/v)溶解,采用Acquity UPLCHSS T3柱(50 mm×2.1 mm,1.8μm)分离,以乙腈-0.05%(v/v)甲酸水溶液为流动相,梯度洗脱,电喷雾正离子模式多反应监测,外标法定量。该方法在0.01～0.3mg/L范围内线性关系良好(r>0.99),在添加含量水平为0.1、0.5、1.0 mg/kg时,平均回收率范围为(84.18±8.04)%～(95.99±6.76)%,相对标准偏差(RSD)为7.04%～10.60%,方法检出限(LOD)为0.8～29μg/kg,方法定量限(LOQ)为2.5～96μg/kg。该方法操作简便、快捷、灵敏、准确,适合棉花中8种脱叶剂的确证和定量测定。A novel method has been developed for the rapid extraction and determination of eight defoliants including thidiazuron, butiphos, methabenzthiazuron, abscisic acid, carfentra- zone-ethyl, diuron, paraquat, and pyrithiobac-sodium in cotton by accelerated solvent extrac- tion （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 （ l ： 9, v/v）. The chro- matographic analysis was performed on an Acquity UPLC 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 spectrome- try 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 defoli- ants at 0. l, 0.5 and 1. 0 mg/kg. The average recoveries of the eight defoliants were from （84. 18± 8.04）% to （95.99±6.75）%. The precision values expressed as RSDs were from 7.04% to l 0.60% （ n = 6）. The limits of detection were 0.8 - 29 μg/kg and the limits of quanti-fication 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 confirma- tion 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 

分 类 号：O658[理学—分析化学]