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作 者:张虹艳 石晓峰[2] 邱国玉 王小乔 许晓辉 潘秀丽 李晨曦 吴福祥 ZHANG Hongyan;SHI Xiaofeng;QIU Guoyu;WANG Xiaoqiao;XU Xiaohui;PAN Xiuli;LI Chenxi;WU Fuxiang(l.Lanzhou Institute for Food and Drug Control,LanZhou 730050;Gansu Academy of Medical Sciences,Lanzhou 730050)
机构地区:[1]兰州市食品药品检验所,兰州730050 [2]甘肃省医学科学研究院,兰州730050
出 处:《分析试验室》2020年第12期1421-1425,共5页Chinese Journal of Analysis Laboratory
基 金:甘肃省药品监督管理局青年科技创新项目(2019GSMPA008)资助。
摘 要:采用热解吸-离子源-原位质谱仪,通过金属探针直接接触面膜表面采集待测物,经热解吸和离子化后,进入三重四极杆质谱检测器以多反应监测模式进行定性分析,实现面膜中6种荧光增白剂(FWAs)的快速检测,并采用高效液相色谱-三重四极杆质谱联用法对该法筛查得到的阳性样品进行验证。结果表明,设置热解吸温度为280℃,以0.1%甲酸水溶液(含10 mmol/L甲酸胺)-乙腈(1:1,V/V)为注射溶剂、注射泵流速为150μL/h时,仪器响应值最优,灵敏度最高;荧光增白剂C.I.135,C.I.162,C.I.185,C.I.367的检出限为2μg/kg;C.I.368,C.I.393的检出限为5μg/kg。应用该法对市售20批次面膜进行检测,1批次检出荧光增白剂C.I.185,C.I.367和C.I.393,与高效液相色谱-三重四极杆质谱联用仪的检测结果一致。方法可用于面膜中荧光增白剂的现场实时快速筛查。A rapid screening method for six fluorescent white agents(FWAs)in facial mask by ambient ionization tandem mass spectrometry was developed.The samples were directly touched by a simple metal probe.The analytes collected on the probe were desorbed and ionized in a thermal desorption electrospray ionization(TD-ESI)source,after that analyte ions were detected by a triple quadruple mass analyzer(QQQ)operated in multiple reaction monitoring(MRM)mode.The results were verified by high performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry(HPLC-MS/MS).The results showed that under the conditions of the temperature of thermal desorption 280℃,0.1%formic acid aqueous solution containing10 mmol/L formic ammonium-acetonitrile(1:1,V/V)as the solvent of injection and the flow rate of 150μL/h,the response of the instrument was the best with the highest sensitivity.The limits of detection(LODs)of C.I.135,C.I.162,C.I.185,and C.I.367 in facial mask were 2μg/kg,and those of C.I.368 and C.I.393 were 5μg/kg.The method was applied to 20 batches of facial mask.FWAs C.I.185,C.I.367 and C.I.393 were detected in one batch,the results were consistent with those obtained by HPLC-MS/MS.This method could be used for rapid qualitative analysis of FWAs in facial mask.
关 键 词:热解吸-离子源-原位质谱法 面膜 荧光增白剂 快速筛查
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