Microextraction Recovery of Tilmicosin Phosphate for HPLC-UV Determination in Washings from Surfaces of Pharmaceutical Equipment

IF 0.8 4区医学 Q4 CHEMISTRY, MEDICINAL Pharmaceutical Chemistry Journal Pub Date : 2024-07-13 DOI:10.1007/s11094-024-03173-3

Z. R. Gizatulina, S. Yu. Garmonov, A. V. Bulatov

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Abstract

A method for microextraction recovery and concentration of tilmicosin phosphate in washings from surfaces of pharmaceutical equipment for its determination by high-performance liquid chromatography with spectrophotometric detection was proposed. The developed method involved dispersion of the extractant (1-dodecanol) in an aqueous solution of a sample while rotating a cotton disk equipped with an inserted magnetic stirrer followed by crystallization of the extract upon cooling the extraction system. The extractant was applied beforehand to the cotton disk. Effective dispersion of the extractant in the aqueous phase during rotation of the cotton disk ensured a high degree of analyte recovery (94%). The detection limit of tilmicosin phosphate (3σ) reached 0.7 mg/L. The determined concentrations ranged from 2 to 250 mg/L. The analytical capabilities of the developed method were demonstrated using quantitative determination of tilmicosin phosphate in washings from surfaces of pharmaceutical equipment after completion of its cleaning as examples.

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微萃取回收磷酸替米考星，用于 HPLC-UV 检测制药设备表面清洗液中的含量

本研究提出了一种微萃取方法，用于回收和浓缩制药设备表面清洗液中的磷酸替米考星，并通过高效液相色谱法和分光光度法进行检测。所开发的方法包括：将萃取剂（1-十二醇）分散在样品的水溶液中，同时旋转装有插入式磁力搅拌器的棉盘，然后在冷却萃取系统后使萃取物结晶。萃取剂事先涂抹在棉盘上。在棉盘旋转过程中，萃取剂在水相中的有效分散确保了分析物的高回收率（94%）。磷酸替米考星（3σ）的检测限为 0.7 mg/L。测定的浓度范围为 2 至 250 mg/L。以制药设备表面清洗后的清洗液中磷酸替米考星的定量测定为例，证明了所开发方法的分析能力。

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来源期刊

Pharmaceutical Chemistry Journal CHEMISTRY, MEDICINAL-PHARMACOLOGY & PHARMACY

CiteScore

1.30

自引率

22.20%

发文量

226

审稿时长

3-8 weeks

期刊介绍： Pharmaceutical Chemistry Journal is a monthly publication devoted to scientific and technical research on the creation of new drugs and the improvement of manufacturing technology of drugs and intermediates. International contributors cover the entire spectrum of new drug research, including: methods of synthesis; results of pharmacological, toxicological, and biochemical studies; investigation of structure - activity relationships in prediction of new compounds; methods and technical facilities used; and problems associated with the development of ecologically safe and economically feasible methods of industrial production. In addition, analytical reviews of the international literature in the field provide coverage of the most recent developments around the world. Pharmaceutical Chemistry Journal is a translation of the Russian journal Khimiko-Farmatsevticheskii Zhurnal. The Russian Volume Year is published in English from April. All articles are peer-reviewed.