色谱

色谱

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气相色谱-质谱法测定茶叶中29种酸性除草剂的残留量

颜鸿飞, 黄志强*, 张莹, 李拥军, 王美玲   

  1. Technology Center, Hunan Entry-Exit Inspection and Quarantine Bureau, Changsha 410004, China
  • 收稿日期:2008-09-04 修回日期:2008-11-04 出版日期:2009-05-30 发布日期:1982-09-25
  • 通讯作者: 黄志强

Determination of 29 acidic herbicide residues in tea by gas chromatography-mass spectrometry

YAN Hongfei, HUANG Zhiqiang*, ZHANG Ying, LI Yongjun, WANG Meiling   

  1. Technology Center, Hunan Entry-Exit Inspection and Quarantine Bureau, Changsha 410004, China
  • Received:2008-09-04 Revised:2008-11-04 Online:2009-05-30 Published:1982-09-25
  • Contact: HUANG Zhiqiang

PDF

937

被引次数

43

摘要： 建立了茶叶中29种酸性除草剂残留量的气相色谱-质谱测定与确证方法。采用乙腈超声振荡提取试样中29种酸性除草剂,石墨化炭黑固相萃取柱净化,三甲基硅烷化重氮甲烷衍生化,再经弗罗里硅土固相萃取柱净化,用气相色谱-质谱法选择离子监测方式测定,外标法定量,根据离子丰度比确证。在加标水平为0.01,0.05,0.1 mg/kg时,29种目标物的加标回收率为57.1%～120.4%,相对标准偏差(RSD)为4.3%～20.9%;方法的检出限在0.002～0.005 mg/kg之间。该方法准确、灵敏、快速,可满足国际上对茶叶中29种酸性除草剂残留的检测需要。

关键词: 茶叶 , 除草剂, 固相萃取, 气相色谱-质谱法, 衍生化

Abstract: A method was developed for the determination of 29 herbicide residues in tea. The target analytes were extracted with acetonitrile. The extract was cleaned up with an ENVI-Carb solid phase extraction column and derivatized with trimethylsilydiazmethan, then cleaned up through a Florisil solid phase extraction column. The derivatives were determined by gas chromatography-mass spectrometry (GC-MS) with selected ion monitoring (SIM) mode. The separation and quantification were achieved using an HP-5MS silica capillary column (30 m×0.25 mm×0.25 μm) with a column temperature gradient from 50 ℃ (held for 1 min) to 160 ℃ at a rate of 4 ℃/min, held for 3 min and then increased to 300 ℃ for 5 min at a rate of 10 ℃/min. The average recoveries of these herbicides at three spiked levels (0.01, 0.05 and 0.1 mg/kg) ranged from 57.1% to 120.4% with the relative standard deviations (RSDs) ranged from 4.3% to 20.9%. The detection limits were from 0.002 mg/kg to 0.005 mg/kg. The method is easy, fast, and more sensitive. It also indicated that this method can meet the requirements for simultaneous determination of 29 herbicides in tea.

Key words: derivatization, herbicides, solid phase extraction (SPE), tea , gas chromatography-mass spectrometry (GC-MS)