液相色谱-串联质谱法检测9种腹泻性贝毒毒素

Determination of 9 kinds of diarrhetic shellfish poisoning toxins by liquid chromatography-tandem mass spectrometry

中文关键词:  海洋贝类  腹泻性贝毒毒素  高效液相色谱-电喷雾串联质谱法

英文关键词:marine shellfish  diarrhetic shellfish poisoning toxins  high performance liquid chromatography-electrospray ionization mass spectrometry

中文摘要:

      目的 建立腹泻性贝毒毒素9种代表性化合物: 大田软海绵酸、鳍藻毒素、蛤毒素2、扇贝毒素及其衍生物、环亚胺米氏裸甲藻毒素、螺环内酯毒素1和原多甲藻酸的高效液相色谱-电喷雾串联质谱(HPLC-ESI-MS/MS)检测方法。方法 以80%甲醇水溶液对贝类组织中的毒素进行提取, 再以亲水亲脂平衡柱(HLB)对提取液进行净化, 最后以高效液相色谱-电喷雾串联质谱测定。结果 DSP毒素9种代表性化合物在各自浓度范围内线性良好, 回收率为68.9%~94.2%, 精密度为3.5%~9.5%。结论 该方法具有灵敏度高、重现性好、操作简便、准确可靠等特点, 适用于贝类中腹泻性贝毒毒素的测定。

英文摘要:

      Objective To establish a high performance liquid chromatography (HPLC)-electrospray ionization mass spectrometry method for determination of 9 kinds of representative diarrhetic shellfish poisoning (DSP) toxins including okadaic acid(OA), dinophysistoxin1, 2(DTX1, DTX2), pectenotoxin2(PTX2), yesso-toxin(YTX), homo-yessotoxin(hYTX), gymnodimine(GYM), spirolide1(SPX1) and azaspiracid1(AZA1) in shellfish. Methods The toxins were extracted with 80% methanol aqueous solution from the shellfish, then cleaned up by hydrophile-lipophile balance columns, at last, the extractive was determined by a reversed phase HPLC gradient program coupled with electrospray ionization mass spectrometry. Results Nine representative diarrhetic shellfish poisoning toxins had a good linear relationship in respective concentration range, the average recoveries were ranged from 68.9%~94.2%, and the precision was in ranged from 3.5%~9.5%. Conclusion The developed method is simple and accurate, which can be applied for determination of DSP toxins in shellfish.