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抗生素化学分析的改进。十一、聚醚类抗生素的同步荧光密度测定法

Improvement of chemical analysis of antibiotics. XI. Simultaneous fluorodensitometric determination of polyether antibiotics.

作者信息

Asukabe H, Yoneyama H, Mori Y, Harada K, Suzuki M, Oka H

出版信息

J Chromatogr. 1987 Jun 19;396:261-71. doi: 10.1016/s0021-9673(01)94063-4.

DOI:10.1016/s0021-9673(01)94063-4
PMID:3624375
Abstract

A simultaneous determination of three polyether antibiotics, salinomycin, monensin and lasalocid, was established by silica gel and RP-18 high-performance thin-layer chromatography (HPTLC) using 18,19-dihydrosalinomycin and 18,19-dihydro-20-ketosalinomycin as internal standards. Fluorescent derivatives of the polyethers were prepared by reaction of their sodium salts with 1-bromoacetylpyrene and Kryptofix 222 in acetonitrile. A silica gel HPTLC plate with carbon tetrachloride-ethyl acetate-acetonitrile (50:5:10) as a solvent system and a RP-18 HPTLC plate with dichloromethane-ethyl acetate-acetone-acetonitrile (15:2:1:55) gave satisfactory separations of the five pyrenacyl esters of salinomycin, monensin, lasalocid, 18,19-dihydrosalinomycin and 18,19-dihydro-20-ketosalinomycin. Under these conditions the internal standard 18,19-dihydrosalinomycin was found to be suitable for the simultaneous determination of salinomycin and monensin, and 18,19-dihydro-20-ketosalinomycin for lasalocid. A linear relationship was obtained between the fluorescence intensity and the amount of each antibiotic in the range 2-14 ng. The detection limit of the three antibiotics was 100 pg.

摘要

采用硅胶和RP - 18高效薄层色谱法(HPTLC),以18,19 - 二氢盐霉素和18,19 - 二氢 - 20 - 酮盐霉素作为内标,建立了同时测定三种聚醚类抗生素盐霉素、莫能菌素和拉沙洛西的方法。聚醚类抗生素的荧光衍生物通过其钠盐与1 - 溴乙酰芘和穴醚222在乙腈中反应制备。以四氯化碳 - 乙酸乙酯 - 乙腈(50:5:10)为溶剂系统的硅胶HPTLC板和以二氯甲烷 - 乙酸乙酯 - 丙酮 - 乙腈(15:2:1:55)为溶剂系统的RP - 18 HPTLC板,能使盐霉素、莫能菌素、拉沙洛西、18,19 - 二氢盐霉素和18,19 - 二氢 - 20 - 酮盐霉素的五种芘甲酰酯得到满意的分离。在这些条件下,发现内标18,19 - 二氢盐霉素适用于同时测定盐霉素和莫能菌素,18,19 - 二氢 - 20 - 酮盐霉素适用于测定拉沙洛西。在2 - 14 ng范围内,荧光强度与每种抗生素的量呈线性关系。三种抗生素的检测限为100 pg。

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