摘要
采用电喷雾萃取电离-串联质谱(EESI-MS/MS)技术,在优化条件下建立了鲜竹沥中二苯并[a,h]蒽(DBA)的快速检测方法。在正离子检测模式下,对离子传输管温度、喷雾电压、电喷雾溶剂流速、样品流速进行优化。以硝酸银的甲醇溶液为电喷雾溶剂,诱导DBA和Ag+形成[DBA+Ag]+、[2DBA+Ag]+等特征离子,再结合碰撞诱导解离技术,最终实现了鲜竹沥中DBA的快速定性定量检测。实验结果表明,DBA在0.1~100μg/L质量浓度范围内线性良好,线性相关系数(r2)为0.998 0,方法检出限(LOD)为0.054μg/L,定量下限(LOQ)为0.179μg/L。该方法对鲜竹沥中DBA的加标回收率为81.5%~87.1%,相对标准偏差为1.9%~3.9%。所建方法具有无需复杂样品预处理、准确度高、可直接快速检测等优点,适用于鲜竹沥中DBA的快速筛查与直接分析,同时也为其他PAHs的检测提供了技术手段。
Utilizing electrospray extraction ionization tandem mass spectrometry(EESI-MS/MS)technology,a rapid detection method for benzo[k]tetraphene(DBA)in fresh bamboo juice extract was developed under optimized working conditions.The experiment was conducted in positive ion de⁃tection mode,with optimization of ion transfer tube temperature,spray voltage,electrospray solvent flow rate,and sample flow rate.By using a methanol solution of silver nitrate as the electrospray sol⁃vent,characteristic ions such as[DBA+Ag]+,[2DBA+Ag]+,etc.,were formed,combined with collision-induced dissociation(CID),to rapidly qualitative and quantitative detection of DBA in fresh bamboo juice.Results demonstrated good linearity of DBA in the concentration range of 0.1-100μg/L,with a linear correlation coefficient(r2)of 0.9980,a method detection limit(LOD)of 0.054μg/L,and a limit of quantitation(LOQ)of 0.179μg/L.The spiked recovery is 81.5%-87.1%for DBA in fresh bamboo juice,with a relative standard deviation of 1.9%-3.9%.Notably,this method offers advantages such as simplified sample preparation,high accuracy,and direct and rap⁃id detection,making it suitable for screening and analyzing DBA in fresh bamboo juice,as well as providing a technical means for the detection of other PAHs.
作者
幸慧玉
周亮
朱腾高
康斯坦丁
刘九梅
陈焕文
方小伟
XING Hui-yu;ZHOU Liang;ZHU Teng-gao;Chingin Konstantin;LIU Jiu-mei;CHEN Huan-wen;FANG Xiao-wei(School of Pharmacy,Jiangxi University of Chinese Medicine,Nanchang 330004,China;Mass Spectrometry Laboratory for BioSample Analysis,Jiangxi University of Chinese Medicine,Nanchang 330004,China;Geophysical&Geochemical Exploration Brigade of Jiangxi,Nanchang 330000,China;Development Research Institute of Testing and Certification Technology,Jiangxi General Institute of Testing and Certification,Nanchang 330052,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2024年第8期1280-1286,共7页
Journal of Instrumental Analysis
基金
江西中医药大学校级科技创新团队发展项目(CXTD22005)
高灵敏数字化生物气溶胶直接分析仪离子源的研制与应用(2023ZDPY003)。
