色谱

色谱 ›› 2013, Vol. 31 ›› Issue (7): 697-702.DOI: 10.3724/SP.J.1123.2012.12038

• 研究论文 • 上一篇    下一篇

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

吴刚1, 董锁拽2, 潘璐璐2, 赵珊红1, 王力君3, 郭方龙3, 李丹3   

  1. 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
  • 收稿日期:2012-12-25 修回日期:2013-01-25 出版日期:2013-07-28 发布日期:2013-07-17
  • 通讯作者: 吴刚
  • 基金资助:

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

Determination of eight defoliant residues in cotton by accelerated solvent extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry

WU Gang1, DONG Suozhuai2, PAN Lulu2, ZHAO Shanhong1, WANG Lijun3, GUO Fanglong3, LI Dan3   

  1. 1. Zhejiang Academy of Science and Technology for Inspection & Quarantine, Hangzhou 310015, China;
    2. Silk Testing Center, Zhejiang Entry-Exit Inspection & Quarantine Bureau, Hangzhou 310012, China;
    3. Zhejiang Lead Product Technology Co., Ltd., Hangzhou 310015, China
  • Received:2012-12-25 Revised:2013-01-25 Online:2013-07-28 Published:2013-07-17

PDF

263

被引次数

16

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, 1.8 μ m)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0.01~0.3 mg/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0.8~29 μ g/kg,方法定量限(LOQ)为2.5~96 μ g/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。

关键词: 超高效液相色谱-串联质谱, 加速溶剂萃取, 棉花, 脱叶剂

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® HSS T3 column (50 mm×2.1 mm, 1.8 μ m) 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 μ g/kg and the limits of quantification were 2.5-96 μ g/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.

Key words: accelerated solvent extraction (ASE), cotton, defoliants, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

中图分类号: