Determination of spiramycin and tilmicosin in meat and fish by LC/MS
Determination of spiramycin and tilmicosin in meat and fish by LC/MS
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DOI：
10.3358/shokueishi.44.150
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发表时间：
2003-06-01
期刊：
影响因子：
--
通讯作者：
Nakazawa, H
中科院分区：
文献类型：
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作者：
Horie, M;Takegami, H;Nakazawa, H
建立了液相色谱-电喷雾电离-质谱（LC/ESI-MS）同时测定肉、鱼中大环内酯类抗生素螺旋霉素和替米考星的方法。用0.2%偏磷酸-甲醇（6：4）从肉和鱼中提取药物，并在Oasis HLB柱（60 mg）上净化提取物。正离子化产生分子相关离子（M +2 H）（2+），新螺旋霉素I、螺旋霉素I和替米考星的m/z分别为350.2、422.3和435.3。LC分离在Capcell Pak MG-C18柱（150 X 2 mm W.）以0.02%甲酸-乙腈为移动的流动相，流速为0.2 mL/min，在此条件下，药物的分子相关离子非常清晰。每种药物的校准曲线在0.05至5 ng范围内呈直线，采用选择离子监测（SIM）。在0.2 μ g/g的添加水平下，肉和鱼中药物的回收率为73.2- 89.2%，精密度高。肉类和鱼类中的药物检测限为0.01 μ g/g。
A simple and reliable method using liquid chromatography-electrospray ionization-mass spectrometry (LC/ESI-MS) has been developed for the determination of the macrolide antibiotics spiramycin and tilmicosin in meat and fish. The drugs were extracted from meat and fish with 0.2% metaphosphoric acid-methanol (6:4), and the extracts were cleaned up on an Oasis HLB cartridge (60 mg). Positive ionization produced the molecular related ions, (M + 2H)(2+), at m/z 350.2, 422.3 and 435.3 for neospiramycin I, spiramycin I and tilmicosin, respectively. The LC separation was performed on a Capcell Pak MG-C18 column (150 X 2 mm W.) with a gradient system of 0.02% formic acid-acetonitrile as the mobile phase at a flow rate of 0.2 mL/min. The molecular-related ions of the drugs were very clear under this condition. The calibration graph for each drug was rectilinear from 0.05 to 5 ng with selected ion monitoring (SIM). The recoveries of the drugs from meat and fish fortified at the level of 0.2 mug/g was 73.2-89.2%, with high precision. The limits of detection of the drugs in meat and fish were 0.01 mug/g.