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| Florisil分散固相萃取-HPLC-MS/MS联用法测定果蔬中氯吡脲的残留 | |
| 引用本文： | 张 燕,舒 平,徐 幸,阚海勋,狄家卫. Florisil分散固相萃取-HPLC-MS/MS联用法测定果蔬中氯吡脲的残留[J]. 食品科学, 2016, 37(6): 216-219. DOI: 10.7506/spkx1002-6630-201606039 |
| 作者姓名： | 张 燕 舒 平 徐 幸 阚海勋 狄家卫 |
| 作者单位： | 大理州质量技术监督综合检测中心，云南 大理 671000 |
| 摘 要： | 采用高效液相色谱-串联质谱法快速测定水果、蔬菜中的氯吡脲残留量。样品经乙腈均质提取，无水硫酸镁和Florisil作为吸附剂净化，经0.22 μm微孔滤膜过滤，用0.1%甲酸溶液和乙腈为流动相梯度洗脱，C18柱分离，采用电喷雾正离子多反应监测模式检测，外标法定量。结果表明，氯吡脲在0.5～40 μg/L质量浓度范围内与峰面积呈良好的线性关系（R＞0.999），定量限为1.0 μg/kg，在添加量为1.0、5.0、20 μg/kg时，平均回收率为85.9%～97.9%，相对标准偏差为2.8%～8.7%（n=6）。该方法分析速度快、灵敏度高、重复性好，适用于水果、蔬菜中氯吡脲残留量的测定。 |
| 关 键 词： | 蔬菜 水果 氯吡脲 高效液相色谱-串联质谱法 |
Determination of Forchlorfenuron Residues in Vegetables and Fruits by Florisil Dispersive Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| ZHANG Yan,SHU Ping,XU Xing,KAN Haixun,DI Jiawei. Determination of Forchlorfenuron Residues in Vegetables and Fruits by Florisil Dispersive Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Food Science, 2016, 37(6): 216-219. DOI: 10.7506/spkx1002-6630-201606039 | |
| Authors: | ZHANG Yan SHU Ping XU Xing KAN Haixun DI Jiawei |
| Affiliation: | Dali State Comprehensive Technical Inspection Center, Dali 671000, China |
| Abstract: | High performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was applied to the rapid determination of residual amounts of forchlorfenuron in vegetables and fruits. The samples were extracted with acetonitrile while stirring, purified with the adsorbents Florisil and anhydrous magnesium sulfate, and filtered through 0.22 μm millipore membrane. The filtrate was separated on a C18 column using gradient elution with a mobile phase consisting of 0.1% formic acid and acetonitrile, detected by electrospray ionization (ESI) in the positive mode using multiple reaction monitoring (MRM), and quantified by an external standard method. The developed method showed a good linear relationship in the range of 0.5–40 μg/L for forchlorfenuron, with a correlation coefficient higher than 0.999. The limit of quantitation (LOQ) for forchlorfenuron was 1.0 μg/kg. The average recovery rates were 85.9%–97.9% at spiked levels of 1.0, 5.0, and 20 μg/kg, with relative standard deviation (RSD, n = 6) ranging from 2.8% to 8.7%. This method is fast, highly sensitivity, repeatable and suitable for the determination of forchlorfenuron residues in vegetables and fruits. |
| Keywords: | vegetables fruits forchlorfenuron high performance liquid chromatography-tandem mass spectrometry |
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