摘要
建立了UPLC-MS/MS检测饲料中5种氨基糖苷类抗生素（链霉素、丁胺卡那霉素、安普霉素、庆大霉素、新霉素）的分析方法,样品用高氯酸溶液酸解及沉淀蛋白质,经MCX固相萃取净化、富集后,以10 mmol/L乙酸胺溶液（含0.1％甲酸）一乙腈作为流动相进行梯度洗脱,采用多反应监测（MRM）模式进行定性和定量分析.5种氨基糖苷类在10～500 ug/L的范围内线性关系良好（r≥0.9989）在10、50、100 μg/kg添加水平下的回收率为74％～93％,RSD（n=6）为3.1％～8.1％,定量限（LOQ）为≤5 μg/kg,该方法精密度好,灵敏度高,能简便、快速、准确地测定饲料中的5种氨基糖苷类抗生素.
An ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）method was developed for the quantitative determination of ive aminogly coside antibiotics （streptomycin, amikacin, apramycin, gentamycin, neomycin） in fodder .Perchloric acid solution was used to acidify the sample and precipitate protein the sample. The sample was purified and concentrated by an HLB mini-column. The separation of the aminogly coside was performed on C18 column, by using gradient elution with acetonitrile and water 0.1% Formic acid. The fluent was detected by MS using ESI （positive ion mode）.The multiple reaction monitoring（MRM）. The calibration curves showed good linearity in the mass concentration range of 10-500 μg/L. With the correction coefficients r≥0.9995.The recoveries of the five aminogly coside ranged from 74 % to 93 % at th spiked levels of 10, 50 and 100 μg/kg. The relative standard deviations （n=6） were between 3. 1 % and 8.1%, The limits of quantification were 5 μg/kg for all the analyses. The method is simple ,rapid, sensitive and accurate.
出处
《广东化工》
CAS
2014年第10期144-145,141,共3页
Guangdong Chemical Industry
