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Time-dependent integrity during storage of natural surface water samples for the trace analysis of pharmaceutical products feminizing hormones and pesticides

机译:天然地表水样品存储过程中随时间变化的完整性可用于药品女性化激素和农药的痕量分析

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摘要

Monitoring and analysis of trace contaminants such as pharmaceuticals and pesticides require the preservation of the samples before they can be quantified using the appropriate analytical methods. Our objective is to determine the sample shelf life to insure proper quantification of ultratrace contaminants. To this end, we tested the stability of a variety of pharmaceutical products including caffeine, natural steroids, and selected pesticides under refrigerated storage conditions. The analysis was performed using multi-residue methods using an on-line solid-phase extraction combined with liquid chromatography tandem mass spectrometry (SPE-LC-MS/MS) in the selected reaction monitoring mode. After 21 days of storage, no significant difference in the recoveries was observed compared to day 0 for pharmaceutical products, while for pesticides, significant losses occurred for DIA and simazine after 10 days (14% and 17% reduction respectively) and a statistically significant decrease in the recovery was noted for cyanazine (78% disappearance). However, the estrogen and progestogen steroids were unstable during storage. The disappearance rates obtained after 21 days of storage vary from 63 to 72% for the feminizing hormones. Overall, pharmaceuticals and pesticides seem to be stable for refrigerated storage for up to about 10 days (except cyanazine) and steroidal hormones can be quite sensitive to degradation and should not be stored for more than a few days.
机译:监测和分析药物和农药等微量污染物需要对样品进行保存,然后才能使用适当的分析方法对其进行定量。我们的目标是确定样品的货架寿命,以确保对超痕量污染物进行正确定量。为此,我们在冷藏条件下测试了包括咖啡因,天然类固醇和精选农药在内的多种药品的稳定性。使用多残留方法,通过在线固相萃取结合液相色谱串联质谱法(SPE-LC-MS / MS)在选定的反应监测模式下进行分析。储存21天后,与药品的第0天相比,回收率没有显着差异,而对于农药,在第10天后DIA和simazine发生了重大损失(分别减少了14%和17%),并且统计学上显着下降在回收率中发现了氰嗪(78%消失)。但是,在储存过程中,雌激素和孕激素类固醇是不稳定的。储存21天后,女性激素的消失率从63%到72%不等。总体而言,药品和杀虫剂似乎可以在冷藏条件下稳定保存约10天(氰嗪除外),而类固醇激素对降解非常敏感,因此不应保存几天以上。

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