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Simultaneous determination of 25 pesticides in Zizania latifolia by dispersive solid-phase extraction and liquid chromatography-tandem mass spectrometry

机译:分散固相萃取-液相色谱-串联质谱法同时测定Z子中的25种农药

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摘要

An improved quick, easy, cheap, effective, rugged, and safe (QuEChERS) method combined with ultrapressure liquid chromatography tandem mass spectrometric method (UPLC-MS/MS) was developed to simultaneously determine 25 pesticides in Zizania latifolia. The samples were extracted with methanol(MeOH) and 0.1% formic acid (80:20, v/v) and cleaned with C18 absorbent and primary-secondary amine (PSA). LC separation was performed on a BEH C18 UPLC column under the condition of gradient elution with the mobile phase consisted of 0.5% formic acid (10 mM ammonium acetate)/MeOH. External standard calibration method with matrix-matched was used for quantification, and good linearity was obtained over a concentration range of 0.5–100 μg/l, with correlation coefficients greater than 0.9901. The limit of detection (LOD) and the limit of quantitation (LOQ) of the 25 pesticides were in the range of 0.2–1.0 µg/kg and 0.5–3.3 µg/kg, respectively. The recoveries ranged from 72% to 118%, and the relative standard deviations (RSDs) were less than 20%. Thus, the proposed method is suitable for the simultaneous determination of 25 pesticides in Z. latifolia.
机译:建立了一种改进的快速,简便,廉价,有效,坚固和安全的方法(QuEChERS)与超压液相色谱串联质谱法(UPLC-MS / MS)相结合,可同时测定Zizania latifolia中的25种农药。样品用甲醇(MeOH)和0.1%甲酸(80:20,v / v)萃取,并用C18吸收剂和伯仲胺(PSA)清洗。在BEH C18 UPLC色谱柱上,在梯度洗脱条件下进行LC分离,流动相由0.5%甲酸(10 mM醋酸铵)/ MeOH组成。采用基质匹配的外标校准方法进行定量,在0.5-100μg/ l的浓度范围内获得了良好的线性,相关系数大于0.9901。 25种农药的检出限(LOD)和定量限(LOQ)分别在0.2-1.0μg/ kg和0.5-3.3μg/ kg的范围内。回收率从72%到118%不等,相对标准偏差(RSD)小于20%。因此,该方法适用于同时测定桔梗中25种农药的方法。

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