采用涡旋辅助盐促液-液微萃取技术与超高效液相色谱/串联质谱联用，建立生物监测人尿液中有机磷农药代谢物的快速灵敏分析方法。
Rapid and sensitive analytical procedure for biomonitoring of organophosphate pesticide metabolites in human urine samples using a vortex-assisted salt-induced liquid-liquid microextraction technique coupled with ultra-high-performance liquid chromatography/tandem mass spectrometry.
机构信息
Department of Medicinal and Applied Chemistry, College of Life Sciences, Kaohsiung Medical University, Kaohsiung City, Taiwan.
Department of Population Medicine, Harvard Medical School and Harvard Pilgrim Health Care Institute, Boston, MA, 02115, USA.
出版信息
Rapid Commun Mass Spectrom. 2020 Apr;34 Suppl 1:e8565. doi: 10.1002/rcm.8565. Epub 2020 Feb 12.
RATIONALE
Organophosphate pesticides (OPPs) are the most commonly used insecticides around the world in various agricultural and domestic practices, and humans are frequently exposed to these hazardous insecticides that can lead to several chronic health effects. Therefore, a fast and sensitive analytical method is required for biomonitoring the markers of OPPs in humans for exposure estimation. In this study, a fast and sensitive analytical procedure was developed for the determination of the metabolites of OPPs in human urine samples.
METHODS
Metabolites of OPPs were extracted from 2 mL of urine sample using a novel vortex-assisted salt-induced liquid-liquid microextraction (VA-SI-LLME) technique, and the preconcentrated metabolites were analyzed by ultra-high-performance liquid chromatography/tandem mass spectrometry (UHPLC/MS/MS). Various factors affecting the efficiency of VA-SI-LLME were thoroughly investigated.
RESULTS
The metabolites of OPPs exhibited very good linearity over the concentration range between 0.05 and 50 ng mL with coefficient (r ) values ranging between 0.9986 and 0.9999. The method showed excellent sensitivity with detection limits ranging from 0.01 to 0.03 ng mL and quantification limits from 0.03 to 0.05 ng mL . The developed method was applied to the analysis of real samples and the recoveries ranged between 85.0 and 114.1% with related standard deviations <5%.
CONCLUSIONS
The results showed the VA-SI-LLME/UHPLC/MS/MS method to be a simple, rapid, sensitive, and selective analytical procedure for the biomonitoring of the metabolites of OPPs in humans. This efficient and cost-effective analytical method could be a potential alternative method for the biomonitoring of the metabolites of pesticides in humans.
原理
有机磷农药（OPPs）是目前全球各种农业和家庭实践中使用最广泛的杀虫剂，人类经常接触这些危险的杀虫剂，会导致多种慢性健康影响。因此，需要一种快速灵敏的分析方法来监测人体中 OPPs 标志物，以进行暴露评估。本研究开发了一种快速灵敏的分析程序，用于测定人尿液样本中 OPPs 代谢物。
方法
使用新型涡旋辅助盐诱导液液微萃取（VA-SI-LLME）技术从 2mL 尿液样品中提取 OPPs 代谢物，并用超高效液相色谱/串联质谱（UHPLC/MS/MS）分析浓缩的代谢物。详细研究了影响 VA-SI-LLME 效率的各种因素。
结果
OPPs 代谢物在 0.05 至 50ngmL 浓度范围内表现出很好的线性关系，相关系数（r）值在 0.9986 至 0.9999 之间。该方法具有优异的灵敏度，检测限范围为 0.01 至 0.03ngmL，定量限范围为 0.03 至 0.05ngmL。所开发的方法用于分析实际样品，回收率在 85.0%至 114.1%之间，相对标准偏差 <5%。
结论
结果表明，VA-SI-LLME/UHPLC/MS/MS 方法是一种简单、快速、灵敏、选择性的分析程序，可用于监测人体中 OPPs 代谢物。这种高效且经济有效的分析方法可能是监测人体中农药代谢物的潜在替代方法。
Zotero 插件