分析化学2017，Vol.45Issue(9)：1389-1396,8.DOI:10.11895/j.issn.0253-3820.170173
超高效液相色谱-串联质谱法检测鸡粪中16种残留抗生素
Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Analysis of 16 Kinds of Residual Antibiotics in Chicken Manure
摘要
Abstract
A sensitive and effective method for determination of 16 kinds of antibiotics, including tetracycline, sulfonamide, fluoroquinolone and macrolide, in livestock and poultry manure using solid phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established.Aiming at the chemical properties and sample impurities of the target, the parameters such as mass spectrum conditions, types of extraction and ultrasonic power were optimized.Finally, the samples were extracted with 50% acetonitrile in phosphate buffer solution (pH =4) for three times, followed by ultrasonic steaming, centrifugal and rotary, dilution, and purified by SAX-HLB.After sample loading, the solid phase was washed with 10 mL of methanol-acetone (80∶20, V/V), evaporated to near dryness at 35℃, and then re-dissolved and vortex mixed in 1 mL of 0.1% formic acid∶methanol (1∶1, V/V).The extracts were analyzed with UPLC-MS/MS and calculated by external standard method based on the monitored product ion.The results indicated that the average spiked recoveries of tetracycline, sulfonamide, fluoroquinolone and macrolide in manure were 56.4%-94.6% with relative standard deviations (RSDs) of 2.6%-19.8%, the LODs (S/N=3) were 0.01-2.50 μg/kg, and the LOQs (S/N=10) were 0.05-7.90 μg/kg.The method was simple with high stability, high sensitivity and good reproducibility, and suitable for the simultaneously determination of many antibiotics in animal and poultry manure.关键词
四环素类/磺胺类/氟喹诺酮类/大环内酯类/固相萃取/超高效液相色谱-串联质谱/畜禽粪便Key words
Tetracycline/Sulfonamide/Fluoroquinolone/Macrolide/Solid-phase extraction/Ultra performance liquid chromatography-tandem mass spectrometry/Animal and poultry manure引用本文复制引用
吴丹,韩梅琳,邹德勋,王旭明,高敏,仇天雷..超高效液相色谱-串联质谱法检测鸡粪中16种残留抗生素[J].分析化学,2017,45(9):1389-1396,8.基金项目
本文系现代农业产业技术体系北京市创新团队专项(No.BAIC04-2017)、国家重点研发计划重点专项(No.2016YFD0800205)、科技部重点研发计划(No.2017YFD0801402)和国家自然科学基金(No.51308022)项目资助.This work was supported by the Natural Science Foundation of Beijing, China (No.BAIC04-2017), the National Science and Technology Major Project of the Ministry of Science and Technology of China (No.2016YFD0800205), Key Research and Development Plan of Ministry of Science and Technology of China(No.2017YFD0801402)and National Natural Science Foundation of China(No.51308022). （No.BAIC04-2017）
