单旋钛萃取和同位素稀释质谱法测定人尿中草甘膦的简单可靠的定量

IF 1.5 4区农林科学 Q2 ENTOMOLOGY

Journal of Pesticide Science Pub Date : 2023-01-01 DOI:10.1584/jpestics.d23-030

Takamitsu Otake, Keisuke Nakamura, Nobuyasu Hanari

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引用次数: 0

摘要

研究了单旋TiO萃取- 9-氟酰甲氧羰基氯(FMOC-Cl)衍生-同位素稀释质谱法(IDMS)测定人尿中草甘膦(Gly)含量的方法并进行了优化。优化条件下，FMOC-Gly的定量限为0.3µg/kg，与前人研究结果相当或更低。在优化的分析条件下，对人尿样品进行尖峰检测，FMOC-Gly的准确率为:尖峰水平为0.5µg/kg时为101.6 ~ 104.9%，尖峰水平为30µg/kg时为99.2 ~ 101.0%。日内重复性和日内重复性均<6.5%。“有”衍生化和“没有”衍生化方法之间验证的峰值测试结果在1µg/kg时具有可比性。本研究结果表明，单旋体TiO萃取和IDMS - FMOC-Cl衍生化是一种准确分析人尿中甘氨酸的方法。

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A simple reliable quantification of glyphosate in human urine using MonoSpin TiO extraction and isotope dilution mass spectrometry

A method of quantifying glyphosate (Gly) in human urine by means of MonoSpin TiO extraction and 9-fluorenylmethoxycarbonyl chloride (FMOC-Cl) derivatization with isotope dilution mass spectrometry (IDMS) was investigated and optimized. The method’s quantification limit under optimized conditions was 0.3 µg/kg for FMOC-Gly, which was comparable to or lower than those described in previous studies. When a spike test using human urine samples was carried out with optimized analytical conditions, the trueness for FMOC-Gly was as follows: 101.6–104.9% for a spike level of 0.5 µg/kg and 99.2–101.0% for a spike level of 30 µg/kg. The intra-day repeatability and inter-day reproducibility were <6.5%. The spike test results for validation between the “with” and “without” derivatization methods were comparable at 1 µg/kg. Our results indicate that using MonoSpin TiO extraction and FMOC-Cl derivatization with IDMS is an accurate method for analyzing Gly in human urine.

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来源期刊

Journal of Pesticide Science 农林科学-昆虫学

CiteScore

4.30

自引率

4.20%

发文量

审稿时长

18-36 weeks

期刊介绍： The Journal of Pesticide Science publishes the results of original research regarding the chemistry and biochemistry of pesticides including bio-based materials. It also covers their metabolism, toxicology, environmental fate and formulation.