色谱

色谱 ›› 2014, Vol. 32 ›› Issue (8): 886-889.DOI: 10.3724/SP.J.1123.2014.04014

• 技术与应用 • 上一篇    下一篇

气相色谱-串联质谱法测定台湾青枣中的炔螨特、戊唑醇和溴螨酯残留

张群, 刘春华, 吴南村, 吴小芳, 黎舒怀   

  1. 中国热带农科院分析测试中心, 海南省热带果蔬产品质量安全重点实验室, 海南 海口 571101
  • 收稿日期:2014-04-08 修回日期:2014-05-26 出版日期:2014-08-08 发布日期:2014-08-01
  • 通讯作者: 张群，E-mail：zhangqun123@zju.edu.cn
  • 基金资助:

    海南省重点科技计划项目（2DXM2014047）.

Determination of propargite, tebuconazole and bromopropylate pesticide residues in Taiwan green jujubes by gas chromatography-tandem mass spectrometry

ZHANG Qun, LIU Chunhua, WU Nancun, WU Xiaofang, LI Shuhuai   

  1. Analysis and Testing Center, Chinese Academy of Tropical Agricultural Sciences, Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables, Haikou 571101, China
  • Received:2014-04-08 Revised:2014-05-26 Online:2014-08-08 Published:2014-08-01

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摘要：

建立了台湾青枣（Zizyphus mauritiana Lam）中炔螨特、戊唑醇和溴螨酯同时测定的气相色谱-串联质谱（GC-MS/MS）分析方法。样品用乙腈匀浆提取，盐析，石墨化炭黑/氨基混合型固相萃取柱净化，乙腈/甲苯（3：1，v/v）洗脱，浓缩定容后检测。目标化合物经SLB-5MS色谱柱（30 m×0.25 mm×0.25 μm）分离，采用三重串联四极杆质谱多反应监测（MRM）模式进行定性定量分析。结果表明，在0.01~0.50 mg/kg添加水平时，3种农药的回收率为75.8%~103.6%，相对标准偏差为1.7%~9.3%（n=5）。方法的线性范围为0.01~0.50 mg/kg，决定系数（R2）>0.99。该方法对炔螨特、戊唑醇和溴螨酯的定量限均为0.01 mg/kg，能满足台湾青枣中炔螨特、戊唑醇和溴螨酯残留检测的要求。

关键词: 气相色谱-串联质谱, 炔螨特, 台湾青枣, 戊唑醇, 溴螨酯

Abstract:

An analytical method was established for the determination of propargite, tebuconazole and bromopropylate in Taiwan green jujubes (Zizyphus mauritiana Lam) by gas chromatography-tandem mass spectrometry (GC-MS/MS). The sample was extracted with acetonitrile from the Taiwan green jujubes after treated with a homogenizer. The organic phase was then separated from water phase by adding NaCl. The extract was further purified on a carbon/NH2 cartridge with elution solvents of acetonitrile/toluene (3:1, v/v). Finally, the target analytes were separated by a capillary gas chromatographic column SLB-5MS (30 m×0.25 mm×0.25 μm). A tandem quadrupole mass spectrometer operated in either full scan mode or in MS/MS mode for multiple reaction monitoring (MRM) was used for the qualitative and quantitative analysis of the constituents, respectively. The results showed that the average recoveries of the three pesticides ranged from 75.8% to 103.6% with the RSDs of 1.7%-9.3% at the spiking levels from 0.01 mg/kg to 0.50 mg/kg (n=5). The calibration curves showed good linearity in the range of 0.01-0.50 mg/kg, with the determination coefficients over 0.99 (R2>0.99). The limits of quantification (LOQs) were 0.01 mg/kg for propargite, tebuconazole and bromopropylate in Taiwan green jujubes. The method is available for the determination of propargite, tebuconazole and bromopropylate pesticide residues in Taiwan green jujubes.

Key words: bromopropylate, gas chromatography-tandem mass spectrometry (GC-MS/MS), propargite, Taiwan green jujubes, tebuconazole

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