CAJ | 학술논문

目的：建立了一种河豚中河豚毒素(TTX)的高效液相色谱－串联质谱检测方法。方法取适量样品,在0.03 mol/L乙酸溶液中均质后超声提取样品中的河豚毒素。粗提液低速离心,取上清液加入等量甲醇充分混匀后进行高速离心。高速离心后上清液过0.22μm滤膜后待测。采用Waters ACQUITY UPLC BEH Amide(2.1 mm×100 mm,1.7μm)色谱分析柱,含0.1%甲酸的MilliQ水及乙腈溶液为流动相,电喷雾正离子模式进行分析。结果河豚毒素在5~1000 ng/mL的范围内线性关系良好,相对回收率为83.3%~93.2%,绝对回收率为47.8%~48.9%,检出限为5μg/kg,定量限为20μg/kg。结论与以往检测TTX的LC-MS/MS方法相比,新建方法操作简单、快速、准确、灵敏并且实验成本低,为河豚中TTX的定量检测提供了有效的实用技术手段。
목적：건립료일충하돈중하돈독소(TTX)적고효액상색보－천련질보검측방법。방법취괄량양품,재0.03 mol/L을산용액중균질후초성제취양품중적하돈독소。조제액저속리심,취상청액가입등량갑순충분혼균후진행고속리심。고속리심후상청액과0.22μm려막후대측。채용Waters ACQUITY UPLC BEH Amide(2.1 mm×100 mm,1.7μm)색보분석주,함0.1%갑산적MilliQ수급을정용액위류동상,전분무정리자모식진행분석。결과하돈독소재5~1000 ng/mL적범위내선성관계량호,상대회수솔위83.3%~93.2%,절대회수솔위47.8%~48.9%,검출한위5μg/kg,정량한위20μg/kg。결론여이왕검측TTX적LC-MS/MS방법상비,신건방법조작간단、쾌속、준학、령민병차실험성본저,위하돈중TTX적정량검측제공료유효적실용기술수단。
Objective To establish a new method for determination of tetrodotoxin (TTX) in puffer fish by high performance liquid chromatography - tandem mass spectrometry.Methods The sample was sonicated after homogenizing with 0.03 mol/L acetic acid solution. After a low-speed centrifugation, the supernatant was mixed with equivalent methanol. With a subsequent high-speed centrifugation, the supernatant was filtered through a 0.22μm membrane filter before injection. LC-MS/MS analysis was conducted by Waters ACQUITY UPLC BEH Amide (2.1mm× 100 mm, 1.7μm) column with the mobile phase of 0.1% formic acid in water and acetonitrile at positive mode.Results There was a good linearity of TTX in the range of 5~1000 ng/mL. The matrix recoveries was 85.8%~93.2% and the absolute recoveries was 47.8%~48.9%. The detection limit is5 μg/kg and the limit of quantification is2 0 μg/kg.Conclusion Compared with the previous methods, the new method is simple, rapid, accurate, sensitive and at low cost for the determination of TTX in aquatic products.