摘要
目的建立固态速溶茶粉中啶虫脒、吡虫啉、灭多威、异丙威、克百威5种农药残留的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)的测定方法。方法样品使用乙腈提取,经N-丙基乙二胺(PSA)/石墨化炭黑/无水硫酸镁填料净化,采用ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,i.d.1.7μm)分离,以乙腈(0.1%甲酸)~0.04%醋酸铵(0.1%甲酸)流动相梯度洗脱,以正离子电喷雾电离(ESI+),多反应监测(MRM)模式检测,采用基质标准曲线外标法定量。结果啶虫脒等5种农药在0~50μg/L浓度范围内线性良好,该方法 5种农药的定量限均能达到0.01 mg/kg,加标水平下的回收率为83.2%~114.1%,相对标准偏差为0.3%~5.7%。结论该方法提取效果好,检测灵敏、简便、快速、高效等优点,能够满足固态速溶茶粉中农残检测的需求。
Objective To establish a method for the detection of 5 kinds of pesticide residues,including acetamiprid,imidacloprid,methomyl,isoprocarb,and carbofuran in instant tea by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The samples were extracted with acetonitrile and then purified by N-propyl ethylenediamine(PSA)/graphitized carbon black/anhydrous magnesium sulfate,and the column was ACQUITY UPLC BEH C18(2.1 mm×100 mm,i.d.1.7 μm),with acetonitrile(0.1% formic acid)-0.04% ammonium acetate(0.1% formic acid) as the mobile phrase through gradient elution.The conditions were positive ions electrospray ionization(ESI+),multiple reaction monitoring mode detection(MRM),and matrix quantitative standard curve external standard method.Results The linear range of 5 kinds of pesticide residue was 0~50 μg/L,the limit of quantitative,standard addition recovery,and relative standard deviation were 0.01 mg/kg,83.2%~114.1% and 0.3%~5.7%,respectively.Conclusion This method with high performance of extracting is highly sensitive,rapid and simple,which can be used to determine the pesticide residues in instant tea.
出处
《食品安全质量检测学报》
CAS
2015年第5期1583-1590,共8页
Journal of Food Safety and Quality
基金
福建省茶叶精深加工产业技术公共服务平台项目~~
关键词
超高效液相色谱-串联质谱法
农药残留
固态速溶茶粉
ultra performance liquid chromatography-tandem mass spectrometry
pesticide residues
solid instant tea powder
