Blanchoud Hélène, Alliot Fabrice, Chen Ningxin, Valdes Danièle
EPHE, PSL University, UMR Metis 7619 (Sorbonne Université, CNRS, EPHE), 4 place Jussieu, 75005 Paris, France.
Sorbonne Université, CNRS, EPHE, UMR 7619 Metis, 4 place Jussieu, 75005 Paris, France.
MethodsX. 2020 Feb 20;7:100824. doi: 10.1016/j.mex.2020.100824. eCollection 2020.
A rapid analysis of pesticides using on-line Solid phase extraction LC MS/MS (Agilent Technology) was performed using only 2-mL water samples. SPE cartridge PLRP-s was used for the pre-concentration sample with methanol elution in back flush. Sensitive transitions and mass spectrometry conditions were optimized by direct infusion of individual standard solutions in a positive electrospray mode. Water samples were spiked with internal standards to compensate the matrix effect. The limit of quantification was calculated to be 20 ng L using the standard deviation of blank analysis injected ten times and uncertainties were estimated at less than 20% on concentrations. This method was validated to study leaching water samples for which only small quantities of water were available.•Only 2 mL water sample was used.•Samples were filtered at 0.2 µm and spiked with individual standard.•Compounds were separated in an 18.5-min elution time using the dynamic MRM program.
使用仅2毫升水样，通过在线固相萃取液相色谱串联质谱法（安捷伦科技）对农药进行快速分析。使用PLRP - s固相萃取柱对样品进行预浓缩，采用反冲甲醇洗脱。通过在正电喷雾模式下直接注入单个标准溶液来优化灵敏跃迁和质谱条件。向水样中加入内标以补偿基质效应。使用十次注入空白分析的标准偏差计算出定量限为20 ng/L，浓度的不确定度估计小于20%。该方法经过验证，用于研究仅能获取少量水样的淋溶水样。
•仅使用2毫升水样。
•样品经0.2 µm过滤并加入单个标准品。
•使用动态多反应监测程序在18.5分钟洗脱时间内分离化合物。
