超高效液相色谱串联质谱法测定果蔬中13 种植物生长调节剂残留量

    Determination of 13 plant growth regulator residues in fruitsand vegetables using ultra performance liquidchromatography tandem mass spectrometry

    • 摘要: 建立了超高效液相色谱串联质谱法同时测定果蔬13 种植物生长调节剂残留量的方法。样品经甲醇水提取,用Shim-pack XR C18 色谱柱(75 mm×2.0 mm,1.6 μm),以乙腈-0.1% 乙酸溶液作为流动相梯度洗脱,采用电喷雾离子化,正、负离子扫描,多反应选择离子监测,基质匹配外标法峰面积定量。矮壮素、多效唑、烯效唑、噻苯隆、赤霉素、2—奈乙酸、氯吡脲、2,4—D、调果酸、4—氯苯氧乙酸、2,4,5—三氯苯氧乙酸、6—BA 和氯苯胺灵在质量浓度1~20 μg/L 范围内线性良好,相关系数 r 均大于0.99,样品在10、20、50 μg/kg 等3 个添加水平的平均回收率为81.2%~106%,变异系数为2.13%~11.8%(n=6),方法的定量限为0.022~16 μg/kg。该方法简便、特异性好,适用于果蔬中13 种植物生长调节剂的检测。

       

      Abstract: To develop a ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method for the determination of 13 plant growth regulator residues in fruits and vegetables. The sample wasextracted with methanol–H2O and the chromatographic separation was performed on the Shim-pack XR C18 column(75 mm × 2.0 mm,1.6 μm),using acetonitrile-0.1% acetic acid as the mobile phase by gradient elution. Themethod applied electrospray ionization in positive and negative multiple reaction monitoring mode and quantifiedwith peak area with matrix-matched external standard method. A good linearity of Chlormequat chloride,Paclobutrazol,Uniconazole,thidiazuron,gibberellic acid 2-naphthaleneacetic acid,Forchlorfenuron,2,4-D,Cloprop,4-Chloroph-enoxyacetic acid,2,4,5-Trichlorophenoxyacetic acid,6-Benzylaminopurine and isopropylN-(3-chlorophenyl)carbamate were in the concentration range of 1.0-20 μg/L with a correlation coefficient above0.99. The average recoveries from three different were with the range of 81.2% to 106% at spiked levels of 10,20,50 μg/kg,and the relative standard deviations were between 2.13% to 11.8%(n=6). The limit of quantification wasin the range of 0.022~16 μg/kg. This method is simple,selectivity and suitable for determination of 13 residues infruits and vegetables.