Citation: | ZHU Shichao, QIAN Zhuozhen, WU Chengye. Determination of 7 macrolide antibiotic residues in aquatic products by HPLC-MS/MS[J]. South China Fisheries Science, 2012, 8(1): 54-60. DOI: 10.3969/j.issn.2095-0780.2012.01.009 |
We developed a high performance liquid chromatography tandem mass spectrometric (HPLC-MS/MS) method for determining 7 macrolide antibiotics [oleandomycin (OLD), erythromycin (ERM), kitasamycin (KIT), josamycin (JOS), spiramycin (SPI), tilmicosin (TIL) and tylosin (TYL)] in aquatic products. The samples were extracted with acetonitrile and cleaned up by neutral alumina and n-hexane; data acquisition was achieved by applying selected reaction monitoring (SRM), and quantification analysis was performed with matrix matched standard calibration curves. The standard curves show good linear between the peak areas and concentrations of 7 macrolides in the range of 1~100 ng · mL -1 (R2>0.995). The average recovery of the drugs fortified in different negative samples at 3 spiked levels of 4 μg · kg-1, 20 μg · kg-1 and 40 μg · kg-1 varies from 75.4% to 108%, and the relative standard deviations vary from 0.665% to 12.9%. The detection limit of the drugs in aquatic products is 1 μg · kg-1 and the quantification limit is 4 μg · kg-1. This simple, sensitive and reproducible method can provide technical support for the determination of 7 macrolide antibiotic residues in aquatic products.
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