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建立了固相萃取-气相色谱-质谱法测定河鲀鱼中河鲀毒素的分析方法。河鲀鱼肉用2%乙酸甲醇溶液提取出河鲀毒素,石油醚脱脂,浓缩蒸干,然后用强碱将河鲀毒素水解成2-氨基-8-羟基-6-羟甲基-喹唑啉(C9生物碱),水解液经过MCX阳离子交换固相萃取柱净化、BSTFA衍生,采用气相色谱-质谱法全扫描方式定性分析,定性离子376,392,407,选择离子扫描方式定量分析,定量离子392。河鲀毒素在0.05～5.0μg/mL范围内具有良好的线性,相关系数R2=0.997 5,样品添加浓度为0.02、0.10、0.50mg/kg,测定6次,方法回收率为64.0%～92.8%,相对标准偏差RSD为5.41%～8.63%,方法检测限为5.0μg/kg。实验结果表明,建立的固相萃取-气相色谱-质谱法方法灵敏度高,净化效果好,定性、定量准确。
A method was developed for the determination of tetrodotoxin in tilapia fish by solid-phase extraction coupled with gas chromatography-mass spectrometry. River tuna fish with 2% acetic acid methanol solution extracted toxins, petroleum ether degreasing, concentrated evaporated to dryness, and then strong alkali hydrolysis of tritoxicillin 2-amino-8-hydroxy-6-hydroxymethyl-quinazoline (C9 alkaloids). The hydrolyzate was purified by MCX cation exchange SPE column and derivatized with BSTFA. Qualitative analysis was performed by gas chromatography-mass spectrometry with full scan. Qualitative ions 376, 392, 407 were quantified by selective ion scan and quantified as ions 392. Toxins had a good linearity in the range of 0.05-5.0 μg / mL, the correlation coefficient R2 = 0.997 5, the concentration of samples was 0.02,0.10,0.50 mg / kg, the determination was 6 times, the recoveries were 64.0% -92.8% , The relative standard deviations RSD 5.41% ~ 8.63%, the detection limit of 5.0μg / kg. The experimental results show that the established SPE-GC-MS method has the advantages of high sensitivity, good purification effect and good qualitative and quantitative accuracy.