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首页> 外文会议>Annual conference of the International Society of Exposure Science >Application of LC-full scan HRMS for non-targeted measurement of urinary biomarkers of exposure to modern pesticides
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Application of LC-full scan HRMS for non-targeted measurement of urinary biomarkers of exposure to modern pesticides

机译：LC全扫描HRMS在接触现代农药的尿液生物标志物非目标测量中的应用

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Background: human exposure to pesticides may occur through various routes, often dominated by food consumption. Human biomonitoring is an alternative to monitoring of residues in food and can bring added value for chemical risk assessment because it can reduce the assumptions regarding consumption rates and it integrates exposures from other sources (e.g. house-hold use) [1]. Most modern pesticides are rapidly metabolised and excreted through urine, which is a frequently used non-invasive matrix for human biomonitoring. Detection of biomarkers of exposure (typically metabolites) by targeted analysis methods such as LC-MS/MS is often not possible because analytical reference standards are not available. Non-targeted measurement by LC-full scan HRMS has substantially improved in the past years in terms of sensitivity and selectivity and offers improved possibilities to screen urine samples for pesticide biomarkers. Objectives: development of a generic non-targeted method for the (tentative) detection of biomarkers of exposure to modern pesticides. Methods: for non-targeted measurement a LC-Q-Orbitrap system was used. Acquisition was done using multiple scan events, to generate data with and without fragmentation (full scan/vDIA). Measurement was performed in positive and negative mode in separate injections. Urine samples were analysed with and without deconjugation, with ultrafiltration as only clean up. The raw data were searched for biomarkers using an exact mass database of ions of potential human metabolites. To demonstrate the feasibility of the approach, urine samples were analysed from a volunteer before and after consumption of strawberries known to contain multiple pesticides. Results: through consumption of the strawberries, the volunteer was exposed to a cocktail of seven pesticides, the amounts varied from 0.17 to 0.86 mg. Metabolites, were tentatively detected in urine for five pesticides. In most cases, multiple metabolites were detected. Deconjugation resulted in (enhanced) detection of the aglycon, supporting the tentative detection of the conjugates. For three metabolites a reference standard was available which allowed full confirmation. The detectability varied widely for the different metabolites and ranged from 2 to 700 times the estimated LOD. The results show that detection of pesticide biomarkers of exposure in urine by non-targeted measurement is feasible, even without availability of reference standards. Obviously, for full identification and quantitative analysis, a reference standard is required. Information on the detectability aids in the selection of the best human biomarker for synthesis of a standard.
机译：背景：人类接触农药的途径可能多种多样，通常以食用食物为主导。人体生物监测是监测食品中残留物的替代方法，可以为化学风险评估带来附加值，因为它可以减少关于消费率的假设，并且可以整合来自其他来源（例如家庭使用）的暴露[1]。大多数现代农药会快速代谢并通过尿液排泄，尿液是人类生物监测中经常使用的非侵入性基质。由于没有可用的分析参考标准，通过目标分析方法（例如LC-MS / MS）检测暴露的生物标志物（通常是代谢物）通常是不可能的。在过去的几年中，通过LC全扫描HRMS进行的非目标测量在灵敏度和选择性方面已得到显着改善，并为筛查尿液样品中的农药生物标志物提供了改进的可能性。目标：开发一种通用的非目标方法，用于（初步）检测接触现代农药的生物标志物。方法：对于非目标测量，使用LC-Q-Orbitrap系统。使用多个扫描事件进行采集，以生成带碎片和不带碎片的数据（全扫描/ vDIA）。在正向和负向模式下分别进样进行测量。尿液样品在有和没有去结合的情况下都进行了分析，只有超滤才可以进行超滤。使用潜在的人类代谢物离子的精确质量数据库在原始数据中搜索生物标记。为了证明该方法的可行性，在食用含有多种农药的草莓之前和之后，对志愿者的尿液样本进行了分析。结果：通过食用草莓，志愿者被暴露于七种农药的混合物中，其含量从0.17到0.86 mg不等。尿中初步检测出五种农药的代谢产物。在大多数情况下，检测到多种代谢产物。解偶联导致（增强）糖苷配基的检测，支持对缀合物的初步检测。对于三种代谢物，可以使用参考标准品，以进行完全确认。不同代谢物的可检测性差异很大，范围是估计LOD的2到700倍。结果表明，即使没有参考标准，通过非目标测量来检测尿液中农药暴露的生物标志物也是可行的。显然，要进行全面鉴定和定量分析，需要参考标准。有关可检测性的信息有助于选择最佳的人类生物标志物以合成标准品。

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