食品科学 ›› 2011, Vol. 32 ›› Issue (6 ): 209-212.doi: 10.7506/spkx1002-6630-201106048

• 分析检测 • 上一篇    下一篇

高效液相色谱-串联质谱法测定水果、蔬菜中赤霉素残留

赵瑛博1,周艳明1,*,忻 雪1,2,王岩松3   

  1. 1.沈阳农业大学分析测试中心 2.沈阳市粮油检测计量所 3.沈阳产品质量监督检验院
  • 收稿日期:2010-06-03 修回日期:2011-01-25 出版日期:2011-03-25 发布日期:2011-03-03
  • 通讯作者: 赵瑛博 E-mail:yb_zhao1979@163.com
  • 基金资助:
    国家标准化管理委员会标准制定项目(2006-1018)

Determination of Gibberellin Residue in Vegetables and Fruits by HPLC-MS/MS

ZHAO Ying-bo1,ZHOU Yan-ming1,*,XIN Xue1,2,WANG Yan-song3   

  1. 1. Analysis Test Center, Shenyang Agricultural University, Shenyang 110866, China;
    2. Institute of Shenyang Grain and Oil Metering, Shenyang 110021, China;
    3. Shenyang Product Quanlity Supervision and Inspection Institute, Shenyang 110022, China
  • Received:2010-06-03 Revised:2011-01-25 Online:2011-03-25 Published:2011-03-03
  • Contact: ZHAO Ying-bo1 E-mail:yb_zhao1979@163.com

摘要: 建立一种快速、灵敏的检测蔬菜水果中赤霉素残留量的高效液相色谱-串联质谱(HPLC-MS/MS)方法。采用甲醇溶液作为提取剂,调节pH值后用乙酸乙酯萃取,有机相浓缩后用C18固相萃取柱净化,净化后的溶液用液相色谱-串联质谱仪检测,外标法定量。结果表明:该方法线性范围为0.01~10.0μg/mL,检测限为0.01μg/mL;在添加浓度0.02~1.0mg/kg范围内,赤霉素的平均回收率在77.0%~100.0%之间,变异系数在3.39%~10.05%之间(n=5)。该方法具有灵敏、准确度高的特点,能够满足限量检测的要求。

关键词: 赤霉素, 残留, 高效液相色谱-串联质谱(HPLC-MS/MS)

Abstract: A rapid and sensitive high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the determination of gibberellin residue in vegetables and fruits was developed. The gibberellin in samples was primarily extracted by methanol solution and further extracted by ethyl acetate after pH adjustment from 3 to 4. The extract was purified by C18 column and detected by HPLC-MS/MS with quantification through an external standard method. Linear range of gibberellin in this determination method was between 0.01μg/mL and 10.0μg/mL, and the detection limit was 0.01 μg/mL. The recovery rates of gibberellin in all samples at a spiked level ranging from 0.02 to 1.0 mg/kg were in the range of 77.0% to 100.0% with a CV of 3.39%-10.05%. The results indicated that this developed method was characteristics of high sensitivity and accuracy as wall as low detection limit, which could meet the requirement of MRL determination.

Key words: gibberellin, residue, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)

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