摘要
建立了超高效液相色谱-串联质谱同时检测水产品中亚甲基蓝及其代谢物天青A、天青B、天青C残留的方法。试样中的残留药物采用离子对试剂提取,正己烷脱脂净化,超高效液相色谱-串联质谱法测定。对前处理及液相色谱分离条件进行了探讨与优化。4种分析物在0.25～50μg/L范围内线性关系良好,相关系数均大于0.999,方法定量下限可达0.5μg/kg。在0.5、1.0、5.0μg/kg范围内,平均加标回收率为80%～91%;相对标准偏差为6.38%～9.41%。方法灵敏、稳定,可满足水产品中亚甲基蓝及其代谢物残留的检测与确证及对药物动力学研究的需要。
An ultra-performance liquid chromatographic method with tandem mass spectrometric detec- tion was developed for determination of methylene blue and its metabolites azure A, azure B, azure C in aquatic products. Based on ion-pair formation with p-toluenesulfonic acid, the analytes were extracted from homogenised tissue by acetonitrile -diehloromethane. The extract was separated on Acquity UPLC BEH C18 column using a gradient elution profile. The analytes were detected by mass spectrometry un- der multiple reaction mode（MRM） and an electrospray ionisation（ESI） source. The experimental con- ditions were optimized. Under the optimal conditions, the calibration curve showed a good linearity in the range of 0. 25 -50 t_~g/L for all analytes with the correlation coefficients of more than 0. 999. The quantitive limits for the analytes were down to 0. 5 μg/kg. The average recoveries from spiked tissue samples at three concentration levels of O. 5, 1.0 and 5.0 μg/kg ranged from 80% to 91% with relative standard deviations of 6. 38%- 9.41%. The method had good sensitivity and stability, and was suitable for the determination of methylene blue and its metabolites residues in aquatic products.
出处
《分析测试学报》
CAS
CSCD
北大核心
2009年第1期32-36,共5页
Journal of Instrumental Analysis
基金
十一五国家科技支撑计划资助项目(2006BAK02A08)
福建省科技攻关重点项目(2006Y0002)
关键词
亚甲基蓝
天青A
天青B
天青C
残留
水产品
超高效液相色谱-质谱联用仪
methylene blue
azure A
azure B
azure C
residues
aquatic products
ultra-performance liquid chromatography- tandem mass spectrometry
