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UPLC-MS/MS 法测定犬血浆中头孢呋辛赖氨酸的快速、灵敏、高通量方法。

A fast, sensitive, and high throughput method for the determination of cefuroxime lysine in dog plasma by UPLC-MS/MS.

机构信息

School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China.

出版信息

Talanta. 2012 Jan 30;89:84-90. doi: 10.1016/j.talanta.2011.11.063. Epub 2011 Nov 26.

DOI:10.1016/j.talanta.2011.11.063
PMID:22284463
Abstract

In order to investigate the preclinical pharmacokinetics of cefuroxime lysine, a fast, sensitive and high throughput UPLC-ESI-MS/MS method has been developed and validated for the quantitative determination of cefuroxime in dog plasma. Cefuroxime and IS phenacetin were extracted from plasma samples by PPT or LLE procedure, and then separated on an ACQUITY UPLC™ BEH C(18) column with an isocratic elution of acetonitrile-0.1% formic acid in 10mM ammonium acetate (40:60, v/v). MRM using the fragmentation transitions of m/z 442 → 364 and 180 → 110 in positive ESI mode was performed to quantify cefuroxime and IS, respectively. The calibration curves were linear over the concentration range of 2-400 μg/ml for PPT and 0.01-5 μg/ml for LLE. The LLOQ was 0.01 μg/ml. The intra- and inter-day precisions in all samples were no more than 8.1%, while the accuracy was within ± 6.2% of nominal values. The method was successfully applied to the evaluation of pharmacokinetic parameters of cefuroxime lysine in beagle dogs.

摘要

为了研究头孢呋辛赖氨酸的临床前药代动力学,建立并验证了一种快速、灵敏、高通量的 UPLC-ESI-MS/MS 方法,用于定量测定犬血浆中的头孢呋辛。头孢呋辛和内标苯乙酮通过 PPT 或 LLE 程序从血浆样品中提取,然后在 ACQUITY UPLC™ BEH C(18)柱上进行分离,采用乙腈-0.1%甲酸在 10mM 乙酸铵中的等度洗脱(40:60,v/v)。采用正离子 ESI 模式下的碎片跃迁 m/z 442→364 和 180→110 进行 MRM,分别定量测定头孢呋辛和内标。PPT 的校准曲线在 2-400 μg/ml 范围内呈线性,LLE 的校准曲线在 0.01-5 μg/ml 范围内呈线性。LLOQ 为 0.01 μg/ml。所有样品的日内和日间精密度均不超过 8.1%,而准确度在标称值的±6.2%范围内。该方法成功应用于评价比格犬头孢呋辛赖氨酸的药代动力学参数。

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