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

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。

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.