CAJ | 학술논문

建立了测定人尿液和血浆中河豚毒素( TTX)的超高液相色谱-三重四极杆质谱联用分析方法。尿液和血浆样品经免疫亲和柱净化,以0.1%甲酸-乙腈和0.1%甲酸溶液作为流动相进行梯度洗脱,在UPLC BEH Amide柱上实现分离,正离子电喷雾多反应监测( MRM)模式检测,溶剂标准外标法定量。尿液和血浆中TTX的测量范围为0.05~400μg/L,平均加标回收率分别为92%~95%和91%~96%,相对标准偏差在3.3%~7.2%和3.9%~7.8%(n=5)之间,样品中 TTX的检出限(S/N=3)均为0.02μg/L,定量限(S/N=10)为0.05μg/L。本方法适用于尿液和血浆中TTX的中毒检测和临床监测。
건립료측정인뇨액화혈장중하돈독소( TTX)적초고액상색보-삼중사겁간질보련용분석방법。뇨액화혈장양품경면역친화주정화,이0.1%갑산-을정화0.1%갑산용액작위류동상진행제도세탈,재UPLC BEH Amide주상실현분리,정리자전분무다반응감측( MRM)모식검측,용제표준외표법정량。뇨액화혈장중TTX적측량범위위0.05~400μg/L,평균가표회수솔분별위92%~95%화91%~96%,상대표준편차재3.3%~7.2%화3.9%~7.8%(n=5)지간,양품중 TTX적검출한(S/N=3)균위0.02μg/L,정량한(S/N=10)위0.05μg/L。본방법괄용우뇨액화혈장중TTX적중독검측화림상감측。
Anultra-performancehydrophilicinteractionliquidchromatography-triplequadrupolemass spectrometric ( UPLC-MS/MS) method was developed for the determination of tetrodotoxin ( TTX) in human urine and plasma. After the sample was cleaned-up and concentrated by immunoaffinity column, the separation of the TTX was carried out on an Acquity UPLC BEH amide column (100 mm×2. 1 mm, 1. 7 μm) with gradient elution using mobile phases of 0. 1% ( V/V) formic acid in water and acetonitrile. The analyte was detected by positive electrospray ionization mass spectrometry in the multiple reaction monitoring ( MRM) mode, and quantified by external solvent standard calibration. The measuring ranges of TTX in urine and plasma were 0. 05-400 μg/L. The average recoveries were 92%-95% and 91%-96% for TTX respectively spiked in urine and plasma with relative standard deviations of 3 . 3%-7 . 2% and 3 . 9%-7 . 8% ( n=5 ) . The limits of detection (LOD, S/N=3) and limits of quantitation (LOQ, S/N=10) of TTX were 0. 02 μg/L and 0. 05μg/L for urine and plasma, respectively. This method is suitable for the detection of TTX in urine and plasma for both forensic and clinical purposes.