高效液相色谱-串联质谱法测定玉米中虫酰肼 残留量

Determination of tebufenozide residue in corn by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  虫酰肼  玉米  高效液相色谱-串联质谱法

英文关键词:tebufenozide  corn  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-串联质谱法检测玉米中虫酰肼的残留量。方法 样品经含1%乙酸的乙腈溶液提取, 再经N-丙基乙二胺(PSA)、石墨化炭黑和十八烷基硅烷(octadecylsilane, ODS)净化, 用 ACQUITY UPLC BEH C18(100 mm×2.1 mm, 1.7 μm)柱分离, 以0.1%乙酸水溶液和乙腈作为流动相进行梯度洗脱, 然后经质谱法检测, 以外标法定量。结果 虫酰肼在4~100 ng/mL浓度范围内时, 线性关系良好, 相关系数为0.9933。在0.001、0.05和25.0 mg/kg 3个水平加标的平均加标回收率为85.5%~105.0%之间, 相对标准偏差均小于10.1%, 检出限为0.001 mg/kg。结论 本方法灵敏准确、操作简便, 可适用于玉米中虫酰肼残留量的测定。

英文摘要:

      Objective To establish a method for detection of worm tebufenozide residue in corn by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Tebufenozide residue in the sample was extracted with acetonitrile containing 1% acetic acid, cleaned up with N-propyl ethylenediamine (PSA), graphitized carbon black and octadecylsilane (ODS), separated by an ACQUITY UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm) using 0.1% acetic acid water solution-acetonitrile as mobile phase for gradient elution, and then detected by tandem mass spectrometry with external standard method for quantification. Results Tebufenozide had a good linearity in the range of 4~100 ng/mL, with a correlation coefficient of 0.9933. The average recoveries of tebufenozide spiked in 3 levels of 0.001, 0.05 and 25.0 mg/kg were ranged from 85.5% to105.0%, with the relative standard deviations below 10.1%. The limit of detection was 0.001 mg/kg. Conclusion This method is sensitive, accurate and simple, which is suitable for the detection of tebufenozide residue in corn.