色谱 ›› 2017, Vol. 35 ›› Issue (11): 1129-1136.DOI: 10.3724/SP.J.1123.2017.07019

• 研究论文 • 上一篇    下一篇

QuEChERS-高效液相色谱-串联质谱法快速测定罗汉果中55种杀菌剂

秦富1, 邓全道2, 李湧1, 黄大新1, 汪文龙1   

  1. 1. 广西出入境检验检疫局检验检疫技术中心, 广西 南宁 530021;
    2. 桂林出入境检验检疫局, 广西 桂林 541004
  • 收稿日期:2017-07-23 出版日期:2017-11-08 发布日期:2014-01-17
  • 通讯作者: 汪文龙,E-mail:1224509828@qq.com
  • 基金资助:

    广西壮族自治区科技创新能力与条件建设计划项目(14123006-15,1598025-1).

Rapid determination of 55 fungicides in siraitia grosvenoriis by QuEChERS and high performance liquid chromatography-tandem mass spectrometry

QIN Fu1, DENG Quandao2, LI Yong1, HUANG Daxin1, WANG Wenlong1   

  1. 1. Inspection and Quarantine Technology Center of Guangxi Entry-Exit Inspection and Quarantine Bureau, Nanning 530021, China;
    2. Guilin Entry-Exit Inspection and Quarantine Bureau, Guilin 541004, China
  • Received:2017-07-23 Online:2017-11-08 Published:2014-01-17
  • Supported by:

    Science and Technology Innovation Capability and Conditional Construction Plan of Guangxi Zhuang Autonomous Region (Nos. 14123006-15, 1598025-1).

摘要:

建立了广西名优特产罗汉果中55种杀菌剂残留的QuEChERS-高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。试样经1%(v/v)醋酸乙腈提取后,加入无水硫酸镁脱水,并使用无水硫酸钠、N-丙基乙二胺(PSA)和C18进行净化。采用均含有0.005 mol/L甲酸铵及0.01%(v/v)甲酸的95%(v/v)乙腈水溶液和水作为流动相中的有机相和水相进行梯度洗脱,在电喷雾离子源正离子模式(ESI+)下采用动态多反应监测(DMRM)进行扫描,基质匹配外标法定量。55种杀菌剂在1.0~100.0 μg/kg范围内线性相关性良好,相关系数(R2)>0.99;方法的检出限(S/N>3)为1.0 μg/kg,定量限(S/N>10)为10.0 μg/kg;加标(10.0 μg/kg)回收率为76.96%~118.45%,相对标准偏差为3.44%~19.63%(n=6)。该法快速、准确、灵敏,适合高通量检测罗汉果中的杀菌剂残留。

关键词: QuEChERS, 动态多反应监测, 高效液相色谱-串联质谱, 罗汉果, 杀菌剂

Abstract:

A method for the determination of 55 fungicides in siraitia grosvenoriis by QuEChERS and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established. The samples were extracted with acetonitrile containing 1%(v/v) acetic acid, then dehydrated by anhydrous magnesium sulfate and purified by anhydrous sodium sulfate, N-propyl ethylenediamine (PSA) and C18. Then, 95% (v/v) acetonitrile aqueous solution (organic phase) and water (aqueous phase), both containing 0.005 mol/L ammonium formate and 0.01% (v/v) formic acid, were used as mobile phases with gradient elution. The compounds were tested by positive electrospray ion source (ESI+) and dynamic multiple reaction monitoring (DMRM) mode. Fifty-five fungicides were quantified by external standard method considering matrix effects. The correlation coefficients (R2) were greater than 0.99, which indicated that the linear dependence of the 55 fungicides were good in the range of 1.0-100.0 μg/kg. The LODs (S/N>3) and LOQs (S/N>10) of all the fungicides were 1.0 μg/kg and 10.0 μg/kg, respectively. The recoveries were in the range of 76.96%-118.45% and the relative standard deviations (RSDs) ranged from 3.44% to 19.63% (n=6). This method has the advantages of rapidity, accuracy and sensitivity for the high-throughput detection of fungicides residues in siraitia grosvenoriis.

Key words: dynamic multi-reaction monitoring (DMRM), fungicides, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), QuEChERS, siraitia grosvenoriis

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