食品科学 ›› 2009, Vol. 30 ›› Issue (10): 176-178.doi: 10.7506/spkx1002-6630-200910037

• 分析检测 • 上一篇    下一篇

超高效液相色谱-质谱法测定蔬菜水果中茚虫威的残留量

江滨炜   

  1. JIANG Bin-wei
  • 收稿日期:2008-07-01 修回日期:2009-01-08 出版日期:2009-05-15 发布日期:2010-12-29
  • 通讯作者: 江滨炜 E-mail:jiangbinwei@163.com

Determination of Indoxacarb Residues in Vegetables and Fruits by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry (UPLC-MS/MS)

(Fujian Fairreach Food Safety Testing Co. Ltd., Fuzhou 350015, China)   

  1. (Fujian Fairreach Food Safety Testing Co. Ltd., Fuzhou 350015, China)
  • Received:2008-07-01 Revised:2009-01-08 Online:2009-05-15 Published:2010-12-29
  • Contact: JIANG Bin-wei E-mail:jiangbinwei@163.com

摘要:

建立蔬菜、水果中的茚虫威残留的超高效液相色谱- 质谱法(UPLC-MS/MS)检测方法。样品经乙腈提取,旋转蒸发仪浓缩,SEP-PAK C18 固体萃取小柱分离净化;采用Waters BEH C18 色谱柱为分离柱,以乙腈-20mmol/L乙酸铵水溶液(含0.1% 甲酸)为流动相,在正离子模式下以电喷雾电离串联质谱仪进行测定。分别加标1.0 μg/kg 和5μg/kg 进行回收实验,平均回收率达90% 以上,平行测试6 次相对标准偏差RSD<5.0%,方法的检出限(S/N=3)为0.05μg/L。

关键词: 茚虫威, 超高效液相色谱-质谱法, 固相萃取, 蔬菜, 水果

Abstract:

A new method was developed with ultra-performance liquid chromatography-tandem mass spectrometry (UPLCMS/MS) to determine indoxacarb pesticide residue in vegetables and fruits. Samples were extracted by acetonitrile and cleaned up on a solid-phase extraction (SPE)-PAK C18 cartridge column. The reconstituted sample solution was analyzed by UPLC-MS/MS under positive ion mode. Waters BEH C18 was taken as the analytical column, and 20 mmol/L ammonium acetate aqueous solution containing 0.1% formic acid-acetonitrile containing 0.1% formic acid was taken as the mobile phase. When fresh cabbage was the matrix, the spike recoveries of indoxacarb were 89.5% to 101.2% (n = 6), and the average recovery was 93.45%. When freezedried cabbage was the matrix, the spike recoveries of indoxacarb were 82.4% to 105.3% (n = 6), and the average recovery was 90. 6%. Both the within-day and inter-day RSDs (n = 6) were less then 5.0%. The detection limit of indoxacarb by this method was 0.05 μg/L (S/N = 3).

Key words: indoxacarb, ultra-performance liquid chromatography-mass spectrometry (UPLC-MS/MS), SPE, vegetables, fruits

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