高效液相色谱-串联质谱法测定玉米中虫酰肼残留量.PDFVIP

第 8卷 第 2期 食品安全质量检测学报 Vol. 8 No. 2 2017年 2月 Journal of Food Safety and Quality Feb. , 2017 *通讯作者: 吕鹏, 工程师, 主要研究方向为食品质量与安全, E-mail: 164352847@ *Corresponding author: LV Peng, Engineer, Heihe Entry-Exit Inspection and Quarantine Bureau, Heihe 164300, China. E-mail: 164352847@ 高效液相色谱-串联质谱法测定玉米中虫酰肼 残留量 吕 鹏 1*, 田 丰 1, 宋文成 1, 杨长志 2, 刘 巍 3 (1. 黑河出入境检验检疫局, 黑河 164300; 2. 黑龙江出入境检验检疫局, 哈尔滨 150001; 3. 同江出入境检验检疫局, 佳木斯 156499) 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。 关键词: 虫酰肼; 玉米; 高效液相色谱-串联质谱法 Determination of tebufenozide residue in corn by high performance liquid chromatography-tandem mass spectrometry LV Peng1*, TIAN Feng1, SONG Wen-Cheng1, YANG Chang-Zhi2, LIU Wei3 (1. Heihe Entry-Exit Inspection and Quarantine Bureau, Heihe 164300, China;2. Heilongjiang Entry-Exit Inspection and Quarantine Bureau, Harbin 150001, China; 3. Tongjiang Entry-Exit Inspection and Quarantine Bureau, Jiamusi 156499, China) ABSTRACT: 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 o