食品科学

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超高效液相色谱-三重四极杆串联质谱法测定木瓜中联苯肼酯及其代谢产物

张 月,韩丙军,赵方方   

  1. 中国热带农业科学院分析测试中心,海南省热带果蔬产品质量安全重点实验室,海南 海口 571101
  • 出版日期:2015-12-25 发布日期:2015-12-24

Determining of Bifenazate and Its Metabolite Residues in Papaya by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

ZHANG Yue, HAN Bingjun, ZHAO Fangfang   

  1. Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables, Analysis and Testing Center,
    Chinese Academy of Tropical Agriculture Science, Haikou 571101, China
  • Online:2015-12-25 Published:2015-12-24

摘要:

建立木瓜中联苯肼酯及其代谢产物联苯肼酯烯的超高效液相色谱-三重四极杆串联质谱分析方法。样品用乙腈和0.25%乙酸溶液匀浆提取,盐析,分取上清液,同时加入0.25%抗坏血酸溶液于离心管中,衍生60 min后待测。目标化合物经Waters ACQUITY UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7 μm)分离,采用三重四极杆串联质谱多反应监测模式进行定性定量分析。结果表明,在1.0~10.0 ng/kg添加量时,联苯肼酯及联苯肼酯烯的回收率分别为86.2%~109.8%和78.3%~97.3%,相对标准偏差分别为4.0%~7.0%和4.5%~8.8%(n=5)。方法的线性范围为0.25~2.0 ng/mL,相关系数(r)为0.999 8。该方法对联苯肼酯的定量限均为1×10-6 mg/kg,能满足木瓜中联苯肼酯的残留检测要求。

关键词: 超高效液相色谱-三重四极杆串联质谱, 木瓜, 联苯肼酯, 联苯肼酯烯, 残留

Abstract:

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the
determination of residues of bifenazate and its metabolite bifenazate-diazene in papaya was established. The sample was
extracted with acetonitrile and acetic acid (0.25%) after being homogenized. The organic phase was then separated from
water phase by adding sodium chloride and derivatized for 60 min after the addition of 0.25%. Finally, the target analytes
were separated by a Waters ACQUITY UPLC BEH C18 column (50 mm × 2.1 mm, 1.7 μm). A tandem quadrupole mass
spectrometer operated in MS/MS mode for multiple-reaction monitoring (MRM) was used for the qualitative and quantitative
analyses of the constituents. The results showed that the average recoveries of bifenazate and bifenazate-diazene ranged
from 78.3% to 109.8% with relative standard deviation (RSDs) of 4.0%–8.8% at spiked levels from 1.0 to 10.0 ng/kg (n =
5). The calibration curves showed good linearity in the range of 0.25–2.0 ng/mL, with correlation coefficient over 0.999 8.
The limit of quantification (LOQ) was 1×10-6 mg/kg for both bifenazate and its metabolite. The method is applicable for the
determination of bifenazate pesticide residues in papaya.

Key words: ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), papaya, bifenazate, bifenazate-diazene, residue

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