中文摘要：

目的建立血浆样品中河豚毒素（TTX）的气相色谱-质谱分析方法。方法采用3％乙酸甲醇溶液提取，Oasis MCX固相柱净化，样品液中加入3mol／LKOH溶液和甲醇、DMF将河豚毒素转化成C9碱，经Oasis HLB固相萃取柱净化、再用硅烷化衍生剂（BSTFA＋TMCS）衍生，用气相色谱-质谱联用法进行定性定量分析鉴定。结果方法定性的特征离子为m／z 318、m／z 376、m／z 392、m／z 407，定量离子为m／z 392；定量测定的线性范围在5ng／ml～200ng/ml，相关系数在0．9998，检出限为1．0ng／ml，定量限为5．0ng／ml，血浆样品加标回收率为82．2％～94．7％，相对标准偏差为7．6％～8．8％。结论建立的分析方法快速、准确、选择性好，可适用于公共卫生突发事件的应急检测和临床中毒病人的诊断确证。

英文摘要：

Objective To develop a highly selective and sensitive method for determination of tetrodotoxin （ TTX ） in human plasma by gas chromatography/mass spectrometry. Methods TTX was extracted from plasma samples with methanol containing 3% acetic acid and cleaned up through Oasis MCX cartridges. Then the compound was converted to 2 -amino -6 -hydroxymethyl -8 -hydroxyquinazoline（ C9 -base） under alkaline conditions and extracted with Oasis HLB extraction cartridge. The C9 - base was analyzed after BSTFA ＋ TMCS derivatization by gas ehromatography/mass spectrometry with SIM mode. Results The characteristic mass spectral peaks of TTX- C9 -TMS were observed at m/z318, m/z376, m/z392, m/z407 and quantitative ion was m/z392. The calibration curve for TTX - C9 - TMS was linear from 5 ng/ml to 200 ng/ml with the correlation coefficient of 0. 9998. The detection limit was 1.0 ng/ml and the limit of quantification was 5.0 ng/ml. The recovery rates and RSD of the TFX - C9 - TMS for spiked plasma samples were 82.2% - 94.7% and 7.6% - 8.8% , respectively. Conclusion The method was selective, reliable and accurate, so it is suitable for emergency detection of public health events and clinical diagnostic confirmation of poisoned cases.