食品科学

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QuEChERS-高效液相色谱-串联质谱法测定果蔬中多效唑残留

孙 星,丁 悦,汪佳蕾,王冬兰,沈 燕,刘贤金*   

  1. 江苏省农业科学院食品质量安全与检测研究所,农业部农产品质量安全控制技术与标准重点实验室,江苏 南京 210014
  • 出版日期:2014-04-25 发布日期:2014-05-13
  • 通讯作者: 刘贤金
  • 基金资助:

    国家自然科学基金面上项目(31071719);江苏省农业科技自主创新资金项目(CX(12)3090)

Determination of Paclobutrazol Residues in Fruits and Vegetables by QuEChERS-High Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry

SUN Xing, DING Yue, WANG Jia-lei, WANG Dong-lan, SHEN Yan, LIU Xian-jin*   

  1. Key Laboratory of Control Technology and Standard for Agro-product Safety and Quality, Ministry of Agricultrue,
    Institute of Food Safety and Inspection, Jiangsu Academy of Agricultural Sciences, Nanjing 210014, China
  • Online:2014-04-25 Published:2014-05-13
  • Contact: LIU Xian-jin

摘要:

采用不同的溶剂,通过液液萃取法结合气-质联机对景芝白干酒中的香气成分进行分析,并通过NIST 11 谱库 检索和保留指数进行了鉴定。结果表明,不同种类和极性的有机溶剂,其萃取出来的成分也不相同。采用正戊烷作为 萃取剂,共发现30 种物质,采用乙醚作为萃取剂,共发现29 种物质,采用二氯甲烷作为萃取剂,共发现35 种物质。 3 种溶剂一共萃取出65 种物质,其中醇类化合物9 种、酯类化合物19 种、酸类化合物11 种、烃类化合物14 种、芳香 族化合物3 种、呋喃类化合物3 种、醛类化合物3 种、酮类化合物1 种、含氮化合物1 种、含硫化合物1 种。

关键词: 高效液相色谱-串联质谱, QuEChERS, 多效唑, 水果, 蔬菜, 残留

Abstract:

A method was developed for the determination of paclobutrazol residues in fruits and vegetables by using
QuEChERS-high performance liquid chromatography-triple quadrupole tandem mass spectrometry (HPLC-MS-MS).
Paclobutrazol residues in fruit samples were extracted with acetonitrile, dehydrated with sodium chloride and anhydrous
magnesium sulfate, cleaned up by dispersive solid phase extraction on primary secondary amine and graphitized carbon
black, and detected by HPLC-MS-MS under a multiple reaction-monitoring mode. The qualitative results were obtained
based on the characteristic m/z 294.2/70.0 and m/z 294.2/125.0, and the quantitative results were based on the characteristic
m/z 294.2/70.0. The recoveries of paclobutrazol were in the range from 79.6% to 94.9% at three spiked levels of 0.05, 0.5
and 1 mg/kg from five fruits and vegetable matrixes (pear, apple, peach, tomato and cucumber), with relative standard
deviations (RSDs) between 3.6% and 11.4%, and the limits of detection were 0.4, 0.5, 0.4, 0.4 and 0.5 μg/kg, respectively.
The method is simple, quick, safe, reproducible and applicable to detect and confirm paclobutrazol residues in fruit and
vegetable samples.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS), QuEChERS, paclobutrazol, fruit, vegetable, residues

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