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当前位置: 首页 > 文章 > 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 2011,32 (10) 232-236
Position: Home > Articles > Simultaneous Determination of 4 Tetracyclines and 3 Epimers in Honey by HPLC Coupled with Tandem MS FOOD SCIENCE 2011,32 (10) 232-236

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

作  者：
刘蓉蓉;吴黎明;周金慧;曾明华
单  位：
安徽农业大学;中国农业科学院蜜蜂研究所
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
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10～500μg/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1μg/kg,金霉素及差向金霉素、强力霉素的检测限为2μg/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)。
译  名：
Simultaneous Determination of 4 Tetracyclines and 3 Epimers in Honey by HPLC Coupled with Tandem MS
作  者：
LIU Rong-rong1,2,WU Li-ming2,ZHOU Jin-hui2,ZENG Ming-hua1(1.School of Animal Science and Technology,Anhui Agricultural University,Hefei 230036,China;2.Bee Research Institute,Chinese Academy of Agricultural Sciences,Beijing 100093,China)
关键词：
high performance liquid chromatography-tandem mass spectrometry;honey;tetracyclines;epimers
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 1μg/kg for oxytetracycline,tetracyclines,4-epitetracycline,4-epioxytetracycline and 2 μg/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.

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