| HPLC-MS/MS法分析乙酰甲喹在海参中的主要代谢物 |
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| 引用本文： | 刘慧慧,任传博,张华威,田秀慧,孙岩,薛敬林,邓旭修,徐英江,宫向红,葛萍,刘飞,张秀珍.HPLC-MS/MS法分析乙酰甲喹在海参中的主要代谢物[J].质谱学报,2015,36(5):417-424. |
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| 作者姓名： | 刘慧慧 任传博 张华威 田秀慧 孙岩 薛敬林 邓旭修 徐英江 宫向红 葛萍 刘飞 张秀珍 |
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| 作者单位： | 1.山东省海洋资源与环境研究院，山东省海洋生态修复重点实验室，山东 烟台264006；2.烟台山水海产有限公司，山东 烟台264006；3.赛默飞世尔科技中国有限公司，中国技术培训中心，上海201306 |
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| 摘 要： | 建立了高效液相色谱-串联质谱（HPLC-MS/MS）法分析乙酰甲喹在海参体壁中可能的代谢产物。采用沉淀法和固相萃取法（SPE）对不同种类的代谢物进行净化和浓缩。以含0.1%甲酸的乙腈和含0.1%甲酸的水为流动相，选取AcquityTMUPLC® BEH C18（2.1 mm×50 mm×1.7 μm）色谱柱对代谢物进行梯度洗脱，以电喷雾离子源（ESI）正离子全扫描模式进行检测。通过将样品的一级和二级子离子与标准品比对，确定乙酰甲喹在海参体壁的代谢物中含有3-甲基喹噁啉-2-羧酸（MQCA），同时检测出3种未知代谢物D2、D3、D4，并推测了代谢物可能的裂解途径。
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| 关 键 词： | 高效液相色谱-串联质谱（HPLC-MS/MS） 乙酰甲喹 海参 代谢物 3-甲基喹噁啉-2-羧酸（MQCA） |
Study on Metabolites of Mequindox in Apostichopusjaponicus by HPLC-MS/MS |
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| LIU Hui-hui,REN Chuan-bo,ZHANG Hua-wei,TIAN Xiu-hui,SUN Yan,XUE Jing-lin,DENG Xu-xiu,XU Ying-jiang,GONG Xiang-hong,GE Ping,LIU Fei,ZHANG Xiu-zhen.Study on Metabolites of Mequindox in Apostichopusjaponicus by HPLC-MS/MS[J].Journal of Chinese Mass Spectrometry Society,2015,36(5):417-424. |
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| Authors: | LIU Hui-hui REN Chuan-bo ZHANG Hua-wei TIAN Xiu-hui SUN Yan XUE Jing-lin DENG Xu-xiu XU Ying-jiang GONG Xiang-hong GE Ping LIU Fei ZHANG Xiu-zhen |
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| Affiliation: | 1.Shandong Province Key Laboratory of Restoration for Marine Ecology, Shandong Marine Resource and Environment Research Institute, Yantai 264006, China;2.Yantai Shanshui Seafood Co. LTD, Yantai 264006, China;3.Thermo Fisher Scientific Technical Training Center China Co. LTD, Shanghai 201306, China |
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| Abstract: | Mequindox and its possible metabolites in body wall of Apostichopusjaponicus were identified by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Acetonitrile extraction and hydrochloric acid hydrolysis-SPE extraction were conducted to extract different kinds of metabolites. Metabolites were separated on an AcquityTM UPLC® BEH C18（2.1 mm×50 mm×1.7 μm）column by gradient elution with acetonitrile-water (containing 0.1% formic acid) as mobile phase, and detected by positive ions electrospray ionization (ESI) mass spectrometry with fullscan-data dependent scan. Through comparison of MS1 and MS2 ions with the reference standard, 3-methyl-quinoxaline-2-carbosylic acid (MQCA) is identified as a metabolite of mequindox in Apostichopusjaponicus. The other identified metabolites include D2, D3, D4, and which the fragmentation pathways are deduced. |
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| Keywords: | high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) mequindox Apostichopusjaponicus metabolite 3-methyl-quinoxaline-2-carbosylic acid (MQCA) |
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