高效液相色谱-串联质谱法测定玉米中虫酰肼残留量

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,1.7μm）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4100 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...

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Published in食品安全质量检测学报 Vol. 8; no. 2; pp. 416 - 420
Main Author 吕鹏 田丰 宋文成 杨长志 刘巍
Format Journal Article
LanguageChinese
Published 黑河出入境检验检疫局,黑河,164300%黑龙江出入境检验检疫局,哈尔滨,150001%同江出入境检验检疫局,佳木斯,156499 2017
Subjects
玉米
虫酰肼
高效液相色谱-串联质谱法
tebufenozide
玉米
虫酰肼
corn
high performance liquid chromatography-tandem mass spectrometry
高效液相色谱-串联质谱法
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Summary: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,1.7μm）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4100 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。
Bibliography: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）
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
ISSN:2095-0381