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采用 LC/UV/MS 法在较宽浓度范围内定量检测大鼠血浆中的氟虫腈及其代谢物氟虫腈砜。

Quantification of fipronil and its metabolite fipronil sulfone in rat plasma over a wide range of concentrations by LC/UV/MS.

机构信息

UMR181, Physiopathologie et Toxicologie Expérimentales, INRA, ENVT, 23 chemin des Capelles, 31076 Toulouse, France.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Jul 15;878(22):1934-8. doi: 10.1016/j.jchromb.2010.05.018. Epub 2010 May 24.

DOI:10.1016/j.jchromb.2010.05.018
PMID:20599175
Abstract

Fipronil is an insecticide extensively used to treat pets, which has been identified as a potential thyroid disruptor in the rat. In this species, fipronil is mainly metabolized to fipronil sulfone and plasma concentrations of fipronil sulfone can be at least 20-fold higher than those of fipronil. Investigations of fipronil and fipronil sulfone exposure in blood remain sparse because of the lack of convenient and suitable analytical methods. We have developed and validated an LC/UV/MS/MS method to quantify both fipronil and fipronil sulfone within a wide range of concentrations in rat plasma. The double detection UV and MS coupled on-line enabled the concentrations to be measured over a 3 Log range (2.5-2500 ng/mL). The volume of sample required for the extraction by solid phase extraction was reduced to 75 microL with a recovery higher than 70%. The two-detection method agreement, evaluated with a Bland-Altman plot, was good for concentrations between 50 and 150 ng/mL. The method was applied to monitor plasma concentrations following a commonly used dosage regimen for the toxicological evaluation of fipronil in rats.

摘要

氟虫腈是一种广泛用于治疗宠物的杀虫剂,已被确定为大鼠潜在的甲状腺破坏剂。在这种物种中,氟虫腈主要代谢为氟虫腈砜,氟虫腈砜的血浆浓度至少比氟虫腈高 20 倍。由于缺乏方便和合适的分析方法,血液中氟虫腈和氟虫腈砜暴露的研究仍然很少。我们已经开发并验证了一种 LC/UV/MS/MS 方法,能够在大鼠血浆的宽浓度范围内同时定量检测氟虫腈和氟虫腈砜。在线联用的双检测 UV 和 MS 使浓度能够在 3 Log 范围内(2.5-2500ng/mL)进行测量。固相萃取的样品体积减少到 75μL,回收率高于 70%。通过 Bland-Altman 图评估的双检测方法的一致性对于 50 至 150ng/mL 之间的浓度非常好。该方法用于监测大鼠中氟虫腈毒理学评价常用剂量方案后的血浆浓度。

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