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    固相萃取-超高效液相色谱-串联质谱法测定果蔬中34种植物生长调节剂的残留量

    UPLC-MS/MS Determination of Residual Amounts of 34 Plant Growth Regulators in Fruits and Vegetables with Solid Phase Extraction

    • 摘要: 提出了固相萃取-超高效液相色谱-串联质谱法同时测定果蔬中34种植物生长调节剂残留量的方法。样品2.000 0 g用乙腈10.0 mL提取,经Oasis PRiME HLB固相萃取柱净化。取流出液5.0 mL,氮气吹至近干,用甲醇(1+9)溶液溶解残渣并定容至1.0 mL。以Waters CSH氟苯基色谱柱为固定相,以甲醇-5 mmol·L-1乙酸铵溶液含0.10%(体积分数)乙酸为流动相进行梯度洗脱,采用电喷雾正、负离子源和多反应监测模式检测,外标法定量。34种植物生长调节剂在一定范围内呈线性关系,检出限(3S/N)为0.01~0.20 μg·kg-1。按标准加入法进行回收试验,回收率为71.0%~115%,测定值的相对标准偏差(n=6)为0.60%~16%。

       

      Abstract: A method was proposed for the simultaneous determination of residual amounts of 34 plant growth regulators in fruits and vegetables by UPLC-MS/MS with solid phase extraction. The sample of 2.000 0 g was extracted with 10.0 mL of acetonitrile and purified by passing through Oasis PRiME HLB solid phase extraction column. The eluate of 5.0 mL was taken and concentrated to dryness by N2-blowing, and the residue was dissolved and made its volume up to 1.0 mL with methanol (1+9) solution. The Waters CSH fluorophenyl chromatographic column was used as stationary phase, and the mixture of methanol and 5 mmol·L-1 ammonium acetate solution containing 0.1% (φ) acetic acid was used as mobile phase for gradient elution. ESI+, ESI- and the mode of multi-reaction monitoring were adopted in MS/MS, and external standard method was used for quantification. Linear relationships of 34 plant growth regulators were found in definite ranges, with detection limits (3S/N) in the range of 0.01-0.20 μg·kg-1. Test for recovery was made by standard addition method, giving results in the range of 71.0%-115%, with RSDs (n=6) ranged from 0.60% to 16%.

       

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