超高效液相色谱-串联质谱检测速溶茶中 啶虫脒等5种农药残留量

Determination of 5 kinds of pesticide residues in instant tea by ultra perfor-mance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  农药残留  固态速溶茶粉

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  pesticide residues  solid instant tea powder

中文摘要:

      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. 1.7 μm)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0~50 μg/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。

英文摘要:

      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.