苹果中杀铃脲残留量的快速测定方法研究
目的 建立苹果中杀铃脲的超高效液相色谱-串联质谱(UPLC-MS/MS)快速测定方法。方法 苹果样品通过乙腈匀浆提取, 用固相萃取小柱净化, 甲醇-二氯甲烷(1:19, v:v)淋洗、洗脱后, 选用C18(100 mm×2.1 mm i.d., 1.7 μm)作为分析柱, 甲醇/1 mmol/L 乙酸铵梯度洗脱, 经高效液相色谱分离, 在多反应监测模式(MRM) 及电喷电离方式(ESI )下串联质谱法进行测定, 基质配标准曲线定量。结果 分析物在0.01~0.50 mg/L范围内有良好的线性关系, 相关系数r>0.99, 空白样品中分析物在添加水平为0.01、0.02、0.05 mg/kg时, 平均回收率在80.0%~84.8%之间, 相对标准偏差为4.9%~8.8%, 定量限为0.005 mg/kg。结论 本方法简单快速、灵敏度高、准确度好, 能满足定量分析的要求。
Objective An ultra performance liquid chromatography-tandem mass spectrometry analysis (UPLC-MS/MS) was established for the determination of the residues of triflumuron pesticide in apple. Me-thods The samples were extracted by ultrasonic extraction with acetonitrile and cleaned with solid-phase extraction. The separation was performed on a C18 column(100 mm×2.1 mm i.d., 1.7 μm), the gradient mobile phase consisting of 1 mmol /L ammonium acetate and methanol. The separation was achieved by UPLC, and then the identification and quantification were performed using MS/MS with multiple-reaction monitoring (MRM) and positive electrospray ionization (ESI ) mode. The matrix-matched external standard calibration curves were used for the quantitative analysis. Results Under the optimum conditions, the method showed a good linearity in the range of 0.005~0.50 mg/L with correlation coefficient over 0.99. The limits of quantitation (LOQ) for the pesticide residue were 0.005 mg/kg. The average recoveries of pesticides residues were 80.0%~84.8% at the spiked levels of 0.01, 0.02 mg/kg and 0.05 mg/kg with relative standard deviations (RSDs) of 4.9%~8.8%. Conclusion The method is sensitive and accuracy and it is suitable for quantitative determination of triflumuron pesticides in apple.
标题：苹果中杀铃脲残留量的快速测定方法研究
英文标题：Methodology for rapid determination of triflumuron residue in apple
作者：
刘春华 1.中国热带农业科学院分析测试中心;2.海南省热带果蔬产品质量安全重点实验室
张群 1.中国热带农业科学院分析测试中心;2.海南省热带果蔬产品质量安全重点实验室
黎舒怀 1.中国热带农业科学院分析测试中心;2.海南省热带果蔬产品质量安全重点实验室
吴小芳 1.中国热带农业科学院分析测试中心;2.海南省热带果蔬产品质量安全重点实验室
中文关键词:苹果,杀铃脲,超高效液相色谱-串联质谱,
英文关键词:apple,triflumuron,ultra performance liquid chromatography-tandem mass spectrometry analysis,
发表日期：2014-03-20
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