CAJ | 학술논문

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。
목적：건립고태속용다분중정충미、필충람、멸다위、이병위、극백위5충농약잔류적초고효액상색보-천련질보(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)적측정방법。방법양품사용을정제취,경 N-병기을이알(PSA)/석묵화탄흑/무수류산미전료정화,채용 ACQUITY UPLC BEH C18색보주(2.1 mm×100 mm, i.d.1.7μm)분리,이을정(0.1%갑산)~0.04%작산안(0.1%갑산)류동상제도세탈,이정리자전분무전리(ESI+),다반응감측(MRM)모식검측,채용기질표준곡선외표법정량。결과정충미등5충농약재0~50μg/L농도범위내선성량호,해방법5충농약적정량한균능체도0.01 mg/kg,가표수평하적회수솔위83.2%~114.1%,상대표준편차위0.3%~5.7%。결론해방법제취효과호,검측령민、간편、쾌속、고효등우점,능구만족고태속용다분중농잔검측적수구。
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.