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超高效液相色谱-串联质谱法同时测定脑脊液中罗哌卡因和 3-羟基罗哌卡因。

Simultaneous Determination of Ropivacaine and 3-Hydroxy Ropivacaine in Cerebrospinal Fluid by UPLC-MS/MS.

机构信息

Institute of Forensic Science, Wenzhou Medical University, Wenzhou 325000, China.

Analytical and Testing Center, School of Pharmaceutical Sciences, Wenzhou Medical University, Wenzhou 325035, China.

出版信息

Biomed Res Int. 2020 Dec 4;2020:8844866. doi: 10.1155/2020/8844866. eCollection 2020.

Abstract

In this paper, a UPLC-MS/MS method was developed for the determination of ropivacaine and its metabolite 3-hydroxy ropivacaine in cerebrospinal fluid. The cerebrospinal fluid was processed by ethyl acetate liquid-liquid extraction. The multiple reaction monitoring (MRM) mode was used for quantitative analysis by monitoring the transitions of m/z 275.3 → 126.2 for ropivacaine, m/z 291.0 → 126.0 for 3-hydroxy ropivacaine, and m/z 290.2 → 198.2 for the internal standard. Standard curves for ropivacaine and 3-hydroxy ropivacaine in cerebrospinal fluid were conducted over the concentration range of 0.2-2000 ng/mL, demonstrating excellent linearity, and the lower limit of quantification was 0.2 ng/mL. The intraday precision of ropivacaine and 3-hydroxy ropivacaine was less than 11%, while the interday precision was less than 7%. The accuracy ranged between 87% and 107%, the average extraction efficiency was higher than 79%, and the matrix effect was between 89% and 98%. The developed method was then applied to a case of suspected poisoning of ropivacaine.

摘要

本文建立了一种 UPLC-MS/MS 法,用于测定脑脊液中的罗哌卡因及其代谢产物 3-羟罗哌卡因。采用乙酸乙酯液液萃取法处理脑脊液。采用多反应监测(MRM)模式,通过监测 m/z 275.3→126.2(罗哌卡因)、m/z 291.0→126.0(3-羟罗哌卡因)和 m/z 290.2→198.2(内标)的离子对进行定量分析。罗哌卡因和 3-羟罗哌卡因在脑脊液中的标准曲线浓度范围为 0.2-2000ng/mL,表现出良好的线性,定量下限为 0.2ng/mL。罗哌卡因和 3-羟罗哌卡因的日内精密度均小于 11%,日间精密度均小于 7%。准确度在 87%至 107%之间,平均提取效率高于 79%,基质效应在 89%至 98%之间。该方法随后应用于一例疑似罗哌卡因中毒的案例。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/788d/7787762/ec0df3b290f2/BMRI2020-8844866.001.jpg

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