引用本文:	高莉媛,王艳龙,陈军辉,王帅,史小星,石洪华,郑立.高效液相色谱-离子阱质谱法测定海洋微藻藻粉中的8种脂溶性毒素[J].海洋科学,2016,40(10):113-119.

【打印本页】【HTML】【下载PDF全文】【查看/发表评论】【下载PDF阅读器】【关闭】

过刊浏览高级检索

本文已被：浏览 1278次下载 1311次	码上扫一扫！
分享到：微信更多字体:加大+\|默认\|缩小-
高效液相色谱-离子阱质谱法测定海洋微藻藻粉中的8种脂溶性毒素
高莉媛¹, 王艳龙¹, 陈军辉¹, 王帅¹, 史小星¹, 石洪华¹, 郑立^1,2
1.国家海洋局第一海洋研究所;2.青岛海洋科学与技术国家实验室, 海洋生态与环境科学功能实验室

摘要:

建立了利用高效液相色谱-电喷雾离子阱质谱(HPLC-ESI-IT-MS)测定海洋微藻藻粉中8种典型脂溶性毒素的分析方法。藻粉样品经超声细胞破碎后, 采用超声波辅助提取法对藻毒素进行提取, 用HPLC-ESI-IT-MS多反应离子监测(MRM)模式对各种毒素(包括大田软海绵酸(OA)、鳍藻毒素1(DTX-1)、扇贝毒素2(PTX-2)、虾夷扇贝毒素(YTX)、原多甲藻酸1(AZA1)原多甲藻酸2(AZA2)、罗环内酯毒素(SPX), 米氏裸甲藻毒素(GYM))进行测定。8种脂溶性藻毒素均在线性范围内线性关系良好(R²均在0.991以上), 检出限均介于0.085～1.315 pg之间, 加标回收率在88.5%～111.4%之间, 方法重复性相对标准偏差(RSD)在4.82%～10.17%范围。应用该方法对利玛原甲藻干藻粉中的毒素进行了测定, 分析结果良好, 说明本方法是海洋微藻藻粉中脂溶性藻毒素测定的有效方法。

关键词: 高效液相色谱-离子阱质谱腹泻性贝毒海洋微藻

DOI：10.11759//hykx20151225002

分类号:

基金项目:山东省自然科学基金(ZR2015PD003); 国家基金委-山东省联合基金项目(U1406403); 国家科技支撑计划项目(2013BAK12B00)

Determination of eight typical lipophilic algae toxins in marine microalgae powder using high-performance liquid chromatography-ion trap mass spectrometry

GAO Li-yuan,WANG Yan-long,CHEN Jun-hui,WANG Shuai,SHI Xiao-xing,SHI Hong-hua,ZHENG Li

Abstract:

A method involving high-performance liquid chromatography coupled with electrospray ionization–ion trap mass spectrometry (HPLC–ESI–IT–MS) was developed to determine eight typical lipophilic algae toxins (okadaic acid (OA), dinophysistoxin-1 (DTX-1), pectenotoxin-2 (PTX-2), yessotoxin (YTX), azaspiracid1, 2 (AZA1, AZA2), spirolidel1 (SPX1), gymnodimine (GYM)) in marine microalgae powder. The powder was extracted using ultrasound-assisted extraction after the algae cell-breaking process was performed using ultrasonication. The crude extracts were then analyzed using HPLC–ESI–IT–MS in the multiple reaction monitoring mode. The results showed that the calibration curve for each lipophilic algae toxin was obtained with a good correlation coefficient (R²>0.991) in its linear concentration. The detection limits of the eight target toxins ranged from 0.85 to 1.315 pg. The average recoveries of these toxins ranged from 88.5% to 111.4% with relative standard deviations in the range of 4.82%–10.17%. The proposed method was applied to determine typical lipophilic algae toxins in marine microalgae powder, and good results were obtained. The results also indicated that this method is a useful tool for determining lipophilic algae toxins in marine microalgae powder.

Key words: High-performance liquid chromatography-ion trap mass spectrometry Diarrhetic shellfish poisoning Marine microalgae