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

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 C_(18)(100 mm×2.1 mm,1.7μm)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/m L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。

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 4100 ng/m L, 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.