Paz Beatriz, Riobó Pilar, Souto María L, Gil Laura V, Norte Manuel, Fernández José J, Franco José M
Unidad Asociada (CSIC-IEO) Fitoplancton Tóxico Instituto Español de Oceanografía, Centro Oceanográfico de Vigo (IEO), Apdo. 1552, 36200 Vigo, Spain.
Toxicon. 2006 Nov;48(6):611-9. doi: 10.1016/j.toxicon.2006.07.011. Epub 2006 Jul 13.
The toxin composition of a culture of the dinoflagellate Protoceratium reticulatum was investigated using LC-FLD, after derivatization with DMEQ-TAD (4-(2-(6,7-dimethoxy-4-methyl-3-oxo-3,4-dihydroquinoxalimylethyl)-1,2,4-triazoline-3,5-dione)). Besides yessotoxin (YTX), the new YTX analogue, glycoyessotoxin A (G-YTXA) was detected in culture medium as well as in cells. The conditions for extraction were optimized and the production profile established. Retention time of the resulting fluorescent G-YTXA adduct was identified by comparison of the appropriate standard. Additionally, both G-YTXA and the DMEQ-TAD-G-YTXA adduct were confirmed by LC-MS showing ion peaks at m/z 1273 M-2Na+H and m/z 1618 M-2Na+H, respectively. The LC-MS(n) displayed a fragmentation pattern similar to that of the YTX series.
在用4-(2-(6,7-二甲氧基-4-甲基-3-氧代-3,4-二氢喹喔啉基乙基)-1,2,4-三唑啉-3,5-二酮)(DMEQ-TAD)衍生化后，使用液相色谱-荧光检测器(LC-FLD)研究了网纹原甲藻培养物的毒素组成。除了虾夷毒素(YTX)外，在培养基和细胞中还检测到了新的YTX类似物——糖基虾夷毒素A(G-YTXA)。优化了提取条件并确定了生产概况。通过与适当标准品比较，确定了所得荧光G-YTXA加合物的保留时间。此外，通过液相色谱-质谱联用(LC-MS)确认了G-YTXA和DMEQ-TAD-G-YTXA加合物，分别显示在m/z 1273 M-2Na+H和m/z 1618 M-2Na+H处的离子峰。液相色谱-串联质谱(LC-MS(n))显示出与YTX系列相似的碎片模式。
