CAJ | 학술논문

目的：建立快速、准确检测红鳍东方豚中河豚毒素(tetrodotoxin, TTX)的高效液相色谱-串联质谱(HPLC-MS/MS)的分析方法。方法样品用0.1%乙酸水溶液超声提取, C18固相萃取柱净化,用亲水性色谱柱ZIC?-cHILIC(150 mm×2.1 mm,3μm)洗脱,乙腈-0.1%甲酸水为流动相。选择正离子多反应监测(MRM)模式,[M＋H]+, m/z 320.3/302.2为定量离子,进行HPLC-MS/MS 测定,外标法定量。结果河豚毒素在5~100 ng/mL的范围内呈良好的线性关系,相关系数为0.9997,回收率为82%~91%,相对标准偏差RSD为5.3%~15.7%,方法的定量限为5 ng/mL。结论该方法快速准确,灵敏度高,适用于红鳍东方豚中河豚毒素的测定。
목적：건립쾌속、준학검측홍기동방돈중하돈독소(tetrodotoxin, TTX)적고효액상색보-천련질보(HPLC-MS/MS)적분석방법。방법양품용0.1%을산수용액초성제취, C18고상췌취주정화,용친수성색보주ZIC?-cHILIC(150 mm×2.1 mm,3μm)세탈,을정-0.1%갑산수위류동상。선택정리자다반응감측(MRM)모식,[M＋H]+, m/z 320.3/302.2위정량리자,진행HPLC-MS/MS 측정,외표법정량。결과하돈독소재5~100 ng/mL적범위내정량호적선성관계,상관계수위0.9997,회수솔위82%~91%,상대표준편차RSD위5.3%~15.7%,방법적정량한위5 ng/mL。결론해방법쾌속준학,령민도고,괄용우홍기동방돈중하돈독소적측정。
Objective To establish an accurate, rapid analytical high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the determination of tetrodotoxin (TTX) in the Fugu rubripes. Methods TTX was extracted from sample by 0.1% acetic acid-water, and then purified by solid-phase extraction with C18 sorbent. The separation was performed on the ZIC?-cHILIC (150 mm×2.1 mm, 3 μm) at 35 ℃ using acetonitrile-0.1% acetic acid-water(90:10, v:v) as mobile phase. Samples were analyzed by HPLC-MS/MS and quantified with the external standard method. Quantification was carried out through tandem mass spectrometry with positive electro-spray ionization (ESI) and multiple reaction monitoring (MRM) at m/z [M+H]+320.3 302.2 for TTX. Results Calibration curve was linear over the TTX concentration range of 5~100 ng/mL (r=0.9997), with the limit of quantification of 5 ng/mL. The recoveries were between 82%and 91%with the relative standard deviations (RSD) ranging from 5.3%to 15.7%. Conclusion The method was shown to be sensitive, rapid and suitable for the determination of TTX in Fugu rubripes.