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HPLC-MS/MS测定多宝鱼和紫菜中的砷甜菜碱

Determination of Arsenobetaine in Turbot and Porphyra by HPLC-MS/MS

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【作者】 滕久委李德良吴庆晖舒永红

【Author】 TENG Jiu-wei,LI De-liang,WU Qing-hui,SHU Yong-hong(Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals,China National Analytical Center(Guangzhou),Guangzhou 510070,China)

【机构】 中国广州分析测试中心广东省化学危害应急检测技术重点实验室

【摘要】 建立了多宝鱼和紫菜中砷甜菜碱的高效液相色谱多级质谱联用(HPLC-MS/MS)分析方法。样品以甲醇-水混合液(体积比1∶1)提取,提取液再经氮吹浓缩。样品溶液在C18柱上以1%(体积分数)甲酸和甲醇梯度洗脱,然后在电喷雾电离正离子模式下进行质谱分析。多反应监测模式下进行检测,标准曲线法定量。定量分析的线性范围为10~700μg/L,检出限为4.1μg/L,鱼和紫菜中的加标回收率分别为95%和68%。该文同时还研究了砷甜菜碱的碰撞裂解机理。

【Abstract】 A high performance liquid chromatography-tandem mass spectrometric method was developed for the determination of arsenobetaine in turbot(Scophthatmus maximus) and porphyra.The samples were extracted with 50 ∶50(by volume)water-methanol.The chromatographic separation was performed on a Phenomenex Luna C18(2)(4.6 × 250 mm,5 μm) column by gradient elution with 1%(by volume)formic acid and methanol.The eluent was then analyzed by the MSD TRAP XCT system(Agilent)with electrospray ionization positive ion mode.The collision-induced dissociation(CID) mechanism of arsenobetaine was discussed.The linear range of the calibration curve under MRM(multiple reaction monitoring) mode was 10-700 μg/L with a detection limit of 4.1 μg/L.Spiked recoveries for turbot and porphyra were 95% and 68%,respectively.

【关键词】 形态分析砷甜菜碱多宝鱼紫菜液相色谱-质谱
【Key words】 Asspeciationarsenobetaineturbots,porphyraHPLC-MS/MS
【基金】 广东省自然科学基金资助项目(5000565);广东省科技计划项目(2004B33001005)
  • 【文献出处】 分析测试学报 ,Journal of Instrumental Analysis , 编辑部邮箱 ,2008年07期
  • 【分类号】TS254.7
  • 【被引频次】9
  • 【下载频次】334
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