【摘要】 目的建立高效液相色谱-串联质谱(HPLC-MS/MS)测定烤鱼片中河豚毒素(TTX)的检测方法。方法样品经1%乙酸超声振荡提取15min,提取液加入4倍量的甲醇沉淀水溶性大分子化合物,离心后将上清液挥干,残留物加1mL甲醇复溶,高速离心后取上清液进行HPLC-MS/MS分析检测。色谱分离于HILIC柱上进行,梯度洗脱。采用电喷雾离子源正离子多反应监测(MRM)模式进行定性和定量检测。结果 TTX在5~1 000ng/mL浓度范围内线性关系良好,相关系数为0.999 3,检出限为16μg/kg,回收率为84.6%~98.1%,相对标准偏差(RSD)3.9%~13.7%。结论该方法选择性强、灵敏度高、处理方法简单,适用用于烤鱼片中河豚毒素的测定。更多还原

【Abstract】 Objective To establish an analytical method for qualitative and quantitative analysis of tetrodotoxin(TTX)in roasted fish fillets using HPLC-MS/MS.Methods Specimens were treated by vortexing and ultrasonic-assist extraction in 1%acetic acid.The extract was added into 4volumes of methanol to precipitate soluble macromolecule compounds.After centrifugation,supernatant was evaporated and the residue was redissolved in 1ml of methanol.After high speed centrifugation the supernatant was subjected by HPLC-MS/MS analysis.Separation was performed on a hydrophilic interaction liquid chromatography(HILIC)column via gradient elution.Electrospray ionization(ESI)source in positive ion mode and multi-reaction monitoring(MRM)was used for qualitative and quantitative analysis.Results TTX showed good lineage in the range of 5~1 000ng/ml,correlation coefficient was 0.999 3.Limit of detection(LOD,S/N=3)was 16μg/kg,recovery efficiency for TTX in roast fish fillet was 84.6%~98.1% with relative standard deviation of 3.9%~13.7%.Conclusion The method established in this study is specific,sensitive,easy to operate,which is suitable for qualitative and quantificative analysis of TTX in roasted fish fillets.更多还原