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高效液相色谱法测定羊血浆和奶中头孢吡肟的含量及其药代动力学研究。

High-performance liquid chromatographic determination and pharmacokinetic study of cefepime in goat plasma and milk after pre-column derivatization with Hg(I).

机构信息

Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Assiut University, Assiut, Egypt.

出版信息

J Sep Sci. 2010 Sep;33(17-18):2599-609. doi: 10.1002/jssc.201000294.

DOI:10.1002/jssc.201000294
PMID:20730834
Abstract

A highly sensitive and selective HPLC method with UV detection was developed for the determination of cefepime in goat plasma and milk. The proposed method was based on the complexation of cefepime with Hg(I) ions that imparts the high selectivity of the proposed method with enhancement of the sensitivity which enabled the analysis of cefepime in complex matrices such as plasma and milk. Detection was performed at 263 nm, using cefuroxime sodium as an internal standard. Chromatographic separation of cefepime and the internal standard was achieved with Aqua RP-C(18) column using methanol/triethylamine-acetate buffer, pH 3.5 (18:82, v/v) as mobile phase at a flow rate of 1 mL/min. Linear detector responses were observed spanning the range of 1.3-20 μg/mL. The LOD for standard cefepime was 0.43 μg/mL, whereas the LOD for cefepime in goat plasma was 0.84 μg/mL and the corresponding value in goat milk was 1.1 μg/mL. No interference from endogenous substances in plasma and milk was observed. The developed HPLC method has been successfully applied for the pharmacokinetic study of cefepime in goat plasma and milk, for the first time, after a single intramuscular injection of 50 mg cefepime/kg body weight.

摘要

建立了一种用于测定山羊血浆和奶中头孢吡肟的高灵敏度和选择性 HPLC 法,并结合紫外检测。该方法基于头孢吡肟与 Hg(I)离子的络合,从而赋予了该方法的高选择性,并增强了检测灵敏度,使头孢吡肟在血浆和奶等复杂基质中的分析成为可能。检测波长为 263nm,采用头孢呋辛钠作为内标。头孢吡肟和内标在 Aqua RP-C(18)柱上以甲醇/三乙胺-乙酸盐缓冲液(pH3.5,18:82,v/v)为流动相,流速为 1mL/min 进行分离。标准头孢吡肟的线性检测范围为 1.3-20μg/mL。头孢吡肟的标准检测限为 0.43μg/mL,而在山羊血浆中的检测限为 0.84μg/mL,在山羊奶中的检测限为 1.1μg/mL。在血浆和奶中未观察到内源性物质的干扰。该 HPLC 法已成功应用于山羊血浆和奶中头孢吡肟的药代动力学研究,这是首次在肌肉注射 50mg/kg 头孢吡肟后进行的研究。

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