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引用本文:   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. 分析化学, 2017, 45(9): 1389-1396. doi:  10.11895/j.issn.0253-3820.170173 [复制]

Citation:   WU Dan, HAN Mei-Lin, ZOU De-Xun, WANG Xu-Ming, GAO Min, QIU Tian-Lei. Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Analysis of 16 Kinds of Residual Antibiotics in Chicken Manure. Chinese Journal of Analytical Chemistry, 2017, 45(9): 1389-1396. doi: 10.11895/j.issn.0253-3820.170173 [复制]

超高效液相色谱-串联质谱法检测鸡粪中16种残留抗生素

通讯作者:  仇天雷, qiutianlei@baafs.net.cn

收稿日期: 2017-03-20

接受日期: 2017-06-24

出版日期: 2017-09-20

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

Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Analysis of 16 Kinds of Residual Antibiotics in Chicken Manure

Corresponding author:  QIU Tian-Lei, qiutianlei@baafs.net.cn

Received Date:  2017-03-20

Accepted Date:  2017-06-24

Published Date:  2017-09-20

Fund Project:  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)

建立了固相萃取-超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测畜禽粪便中四环素类、磺胺类、氟喹诺酮类和大环内酯类16种抗生素的分析方法。针对目标物化学性质和样品杂质情况,对质谱条件、提取液种类、超声功率等参数进行了优化。最终以50%乙腈(V/V)的磷酸盐缓冲溶液(pH=4)提取3次,经过超声、离心、旋蒸、稀释后,SAX-HLB串联小柱净化富集,用10 mL甲醇-丙酮混合液(80:20,V/V)洗脱,35℃氮吹近干后,用含0.1%甲酸-甲醇(1:1,V/V)定容,在UPLC-MS/MS多反应检测模式下进行定性及定量分析。结果表明,粪便中四环素类、磺胺类、氟喹诺酮类和大环内酯类抗生素的平均加标回收率为56.4%-94.6%,相对标准偏差(RSD)在2.6%-19.8%之间,方法检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.01-2.50 μg/kg和0.05-7.90 μg/kg。本方法简便、稳定性好、灵敏度高、重现性好,适用于畜禽粪便中多种抗生素的同时检测。

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
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超高效液相色谱-串联质谱法检测鸡粪中16种残留抗生素

吴丹, 韩梅琳, 邹德勋, 王旭明, 高敏, 仇天雷

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