干旱区生态环境知识资源中心(Arid): 液相色谱-串联质谱法同时测定蜂蜜中4种四环素族抗生素及其3种差向异构体

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	液相色谱-串联质谱法同时测定蜂蜜中4种四环素族抗生素及其3种差向异构体
其他题名	Simultaneous Determination of 4 Tetracyclines and 3 Epimers in Honey by HPLC Coupled with Tandem MS
	刘蓉蓉 1; 吴黎明 2; 周金慧 2; 曾明华 1
来源期刊	食品科学
ISSN	1002-6630
出版年	2011
卷号	32 期号:10 页码:232-236
中文摘要	采用液相色谱-质谱联用技术,建立同时测定蜂蜜样品中4种四环素族抗生素及其3种差向异构体的方法。蜂蜜样品中残留的药物用EDTA-McIlvaine缓冲液提取,提取液依次经OASIS HLB及羧酸弱阳离子柱固相萃取柱富集、净化后,用流动相洗脱。洗脱液经微孔滤膜过滤,用流动相甲酸水-乙腈梯度分离,电喷雾-串联质谱进行测定。在多反应监测模式下,22min内7种药物基本实现分离以及定性定量。样品在10～500mug/kg添加范围内,回收率均在64.9%～91.0%之间,相对标准偏差(RSD)不大于10.5%。土霉素及差向土霉素、四环素及差向四环素的检测限为1mug/kg,金霉素及差向金霉素、强力霉素的检测限为2mug/kg。本方法灵敏、可靠,可用于蜂蜜中7种四环素类抗生素的同时检测(其中包括3种毒性代谢产物)。
英文摘要	A method for simultaneous determination of 4 tetracyclines and 3 epimers in honey samples was developed by high performance liquid chromatography coupled with tandem mass spectrometry.The residues in honey samples were extracted by EDTA-Mcllvaine buffer,and cleaned up and condensed by OASIS hydrophilic-liphophilic balance(HLB)column and weak cation exchange(WCX and carboxylic acid)sequentially.Sample solution eluted from the WCX SPE column by mobile phase was filtered by micro-pours membrane,separated by LC-MS/MS with gradient elution using acetonitrile-formic acid solution as mobile phase and then qualitatively and quantitatively analyzed by ESI-MS/MS in a MRM mode.Baseline separation of 7 target drugs was achieved within 7 min,and qualitative and quantitative analysis was completed.The recovery rates of the spiked samples at trace levels were in the range of 64.9% to 91.0% with the relative standard deviation(RSD)less than 10.5%(n = 7).The detection limits were 1mug/kg for oxytetracycline,tetracyclines,4-epitetracycline,4-epioxytetracycline and 2 mug/kg for chlortetracycline,doxycycline and epichlortetracycline.The developed method was sensitive and reliable,and can be successfully applied to the simultaneous detection of 7 target tetracyclines residues including toxic metabolites in honey.
中文关键词	液相色谱-串联质谱法 ; 蜂蜜 ; 四环素类抗生素 ; 差向异构体
英文关键词	high performance liquid chromatography-tandem mass spectrometry honey tetracyclines epimers
语种	中文
国家	中国
收录类别	CSCD
WOS类目	FOOD SCIENCE TECHNOLOGY
WOS研究方向	Food Science & Technology
CSCD记录号	CSCD:4227430
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/227021
作者单位	1.安徽农业大学动物科技学院, 合肥, 安徽 230036, 中国; 2.中国农业科学院蜜蜂研究所, 北京 100093, 中国
推荐引用方式 GB/T 7714	刘蓉蓉,吴黎明,周金慧,等. 液相色谱-串联质谱法同时测定蜂蜜中4种四环素族抗生素及其3种差向异构体[J],2011,32(10):232-236.
APA	刘蓉蓉,吴黎明,周金慧,&曾明华.(2011).液相色谱-串联质谱法同时测定蜂蜜中4种四环素族抗生素及其3种差向异构体.食品科学,32(10),232-236.
MLA	刘蓉蓉,et al."液相色谱-串联质谱法同时测定蜂蜜中4种四环素族抗生素及其3种差向异构体".食品科学 32.10(2011):232-236.