河豚鱼中河豚毒素的气相色谱质谱法测定  

Determination of tetrodotoxin in globefish by gas chromatographymass spectrometry

作　　者：吴平谷[1] 赵永信[1] 沈向红[1] 张晶[1] 王立媛[1] 谭莹[1] 冯靓[1] 

机构地区：[1]浙江省疾病预防控制中心,杭州310009

出　　处：《中国卫生检验杂志》2009年第3期549-551,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的：建立河豚鱼中河豚毒素的气相色谱-质谱法定性、定量测定方法。方法：河豚鱼肉、内脏等用2%乙酸/甲醇提取出河豚毒素,正己烷脱脂,然后用碱将河豚毒素水解成2-氨基-8-羟基-6-羟甲基-喹唑啉（C9碱）,水解液经过C18、SLH固相萃取柱净化、BSTFA衍生,采用气相色谱-质谱法全扫描方式测定,定量离子392。结果：样品添加0.25、1.0、5.0 mg/kg河豚毒素,方法回收率为51.2%～87.0%,RSD为4.7%～6.6%,方法最低检测限为0.05 mg/kg。结论：建立的方法灵敏度高,定性定量准确,完全满足样品检测要求。Ojbective：A method of gas chromatography-mass spectrometry to determine tetrodotoxin in globefish was established.Methods：Extracted with 2% acetic acid/methanol,defatted using hexane.Then alkaline hydrolysis was performed to change tetrodotoxin into 2-amino-6-hydroxymethyl8-hydroxyquinazoline（C9-base）.Further cleanup using C18 cartridge and the purified residue was derivatized with BSTFA,the trimethylsilylated（TMS） C9-base quantitied using scan mode by GC/MS,Quantitied ion was 392.Results：In this way,the rates of recovey of tetrodotoxin were 51.2%～87.0%.The variation coefficients were 4.7%～6.6% when spiked with 0.25,1.0,5.0 mg/kg of the tetrodotoxin and the detection limit of tetrodotoxin was 0.05 mg/kg,respectively.Conclusion：The method of tetrodotoxin detection in globefish is simple,sensitive,accurate and it can be satifactorily applied to the sample analysis.

关 键 词：河豚毒素 气相色谱-质谱法 测定 

分 类 号：O657.71[理学—分析化学]