液相色谱/质谱法测定肉类和鱼类中红霉素和夹竹桃霉素的含量

M. Horie, R. Ishii, Terumitsu Yoshida, Youji Hoshino, H. Nakazawa
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引用次数: 9

摘要

建立了液相色谱-电喷雾-质谱联用(LC/MS-ESI)快速测定肉类和鱼类中大环内酯类抗生素红霉素和夹竹桃霉素的方法。色谱柱为TSK-gel ODS 80-Ts (150×2mm),流动相为0.1%醋酸-乙腈(65:35),流速为0.2mL/min。正电离产生典型的(M+H)+分子离子(红霉素M /z 734;夹竹桃霉素m/ z688)。在选择离子监测(SIM)下,红霉素和夹竹桃霉素在0.05 ~ 10ng范围内呈直线关系。用0.1%偏磷酸-甲醇(5:5)提取药物,用OASIS HLB药筒(60mg)清洗。在0.2μg/g水平下,加样回收率为79.4 ~ 95.4%,精密度高。两种药物在肉类和鱼类中的定量限均为0.01μg/g。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Determination of Erythromycin and Oleandomycin in Meat and Fish by LC/MS
A simple and rapid method using liquid chromatography-electrospray ionization-mass spectrometry (LC/MS-ESI) has been developed for the determination of macrolide antibiotics, erythromycin and oleandomycin, in meat and fish. The LC separation was carried out on a TSK-gel ODS 80-Ts column (150×2mm) by using 0.1% acetic acid-acetonitrile (65:35) as the mobile phase at a flow rate of 0.2mL/min. The positive ionization produced typical (M+H)+ molecular ions of both drugs (erythromycin m/z 734; oleandomycin m/z 688). The calibration graphs for erythromycin and oleandomycin were rectilinear from 0.05 to 10ng with selected ion monitoring (SIM). The drugs were extracted with 0.1% metaphosphoric acid-methanol (5:5), and the extracts were cleaned up on an OASIS HLB cartridge (60mg). The recoveries of the drugs from meat and fish fortified at a level of 0.2μg/g were 79.4-95.4%, with high precision. The limits of quantification of both drugs in meat and fish were 0.01μg/g.
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