色谱

色谱

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高效液相色谱-串联质谱法测定葡萄中的吡效隆和赤霉素

张军1*, 杜平2   

  1. 1. 新疆农业职业技术学院, 新疆 昌吉 831100; 2. 新疆中基天然植物纯化高新技术研究院, 新疆 乌鲁木齐 830088
  • 收稿日期:2011-06-13 修回日期:2011-08-24 出版日期:2011-11-28 发布日期:2011-12-25
  • 通讯作者: 张军,硕士,主要从事食品科学方面的研究
  • 基金资助:

    新疆农业科学基金项目(2008A-11).

Determination of forchlorfenuron and gibberellin acid in the grapes using high performance liquid chromatography-tandem mass spectrometry

ZHANG Jun1*, DU Ping2   

  1. 1. Xinjiang Agricultural Vocational Technical College, Changji 831100, China; 2. Xinjiang Chalkis Natural Plant High-Tech Institute, Urumqi 830088, China
  • Received:2011-06-13 Revised:2011-08-24 Online:2011-11-28 Published:2011-12-25

PDF

643

被引次数

35

摘要： 采用高效液相色谱-串联质谱法（HPLC-MS/MS）建立了葡萄果实中吡效隆（CPPU）和赤霉素（GA3）两种植物生长调节剂残留量的定性定量分析方法。样品用0.5%甲酸水溶液和乙腈（体积比4:1）混合溶剂提取，经Strata-X固相萃取净化，使用Agilent SB-C18 色谱柱（50mm×2.1mm，1.8μm），以0.5%甲酸水溶液-乙腈为流动相，流量0.3mL/min，采用电喷雾离子化源（ESI）多反应监测（MRM）模式下HPLC-MS/MS检测。在最佳检测条件下，得到吡效隆和赤霉素在2.0～100.0μg/L检测范围内线性关系良好，相关系数大于0.999；检出限(LOD)分别为0.3μg/L、0.5μg/L，定量限(LOQ)分别为1.0μg/L、2.0μg/L，回收率和精密度均能达到要求，表明该法准确，可用于葡萄中吡效隆和赤霉素残留量测定。

关键词: 吡效隆, 赤霉素, 高效液相色谱-串联质谱, 葡萄

Abstract: A method was established for the determination of two plant growth regulators, forchlorfenuron (CPPU)and gibberellin acid (GA3), in the grapes using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was extracted with 0.5%(v/v) formic acid aqueous solution and acetonitrile (4:1, v/v), and cleaned-up with Strata-X solid phase extraction cartridge. The separations were performed on an Agilent SB-C18 column (50 mm×2.1 mm, 1.8 μm), with a mobile phase of 0.5% formic acid aqueous solution-acetonitrile at a flow rate of 0.3 mL/min and detected by electrospray ionization MS/MS under the multiple reaction monitoring (MRM) mode. The results showed that the good linear relationships and the correlation coefficients greater than 0.999 were obtained. The limits of detection (LODs) were 0.5 μg/L and 0.3 μg/L for CPPU and GA3, respectively. The limits of quantification (LOQs) were 2.0 μg/L and 1.0 μg/L for CPPU and GA3, respectively. The recoveries were 91.7%~95.6% and 90.3%~94.2% with the relative standard deviations (RSD) of 4.1%~7.3% and 3.2%~6.9% for CPPU and GA3, respectively. The results indicate that the method is accurate and can be used for the determination of CPPU and GA3 residues in the grapes.

Key words: forchlorfenuron (CPPU), gibberellin acid (GA3), grape, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)