基于高分辨质谱技术的儿童口罩中荧光增白剂非靶向筛查鉴定  

Non-Target Screening and Identification of Fluorescent Whitening Agents in Children Masks Based on High Resolution Mass Spectrometry

作　　者：罗忻 王振聚 谢堂堂 丁友超 汤志旭 叶曦雯 牛增元 LUO Xin;WANG Zhen-Ju;XIE Tang-Tang;DING You-Chao;TANG Zhi-Xu;YE Xi-Wen;NIU Zeng-Yuan(Technology Center of Qingdao Customs District,Qingdao 266109,China;College of Chemistry and Chemical Engineering,Ocean University of China,Qingdao 266100,China;The Testing and Technology Center for Industrial Products,Shenzhen Customs,Shenzhen 518000,China;Nanjing Customs District Industrial Products Inspection Center,Nanjing 210001,China)

机构地区：[1]青岛海关技术中心,青岛266109 [2]中国海洋大学化学化工学院,青岛266100 [3]深圳海关工业品检测技术中心,深圳518000 [4]南京海关工业产品检测中心,南京210001

出　　处：《分析化学》2021年第11期1926-1936,共11页Chinese Journal of Analytical Chemistry

基　　金：国家重点研发计划项目(No.2016YFF0203702);海关总署科研项目(No.2019HK070)资助

摘　　要：荧光增白剂(Fluorescent whitening agents,FWAs)是一类荧光染料,广泛应用于纺织品、纸张、洗涤剂、化妆品、塑料玩具和食品接触材料等产品。FWAs对人体和环境具有危害性。本研究建立了基于高效液相色谱-高分辨质谱技术非靶向筛查鉴定7类31种FWAs的方法,并分析了18个品牌的儿童口罩。以甲醇-水(3∶1,V/V)混合溶液为提取溶剂,超声辅助萃取儿童口罩中的FWAs,流动相为甲醇和5 mmol/L乙酸铵溶液,梯度洗脱分离,采用全扫描+数据依赖性扫描模式进行高分辨质谱检测。基于化合物精确分子量、母离子同位素丰度比、预测保留时间和预测碎片离子等多维信息进行定性确证,使用Xcalibur、Mass Frontier和ACD/MS Fragmenter软件对检出的3个儿童口罩中的4种FWAs进行碎片结构推导,将结果与文献报道比对。通过FWAs的标准品进行了准确的定性与定量分析,并采用代表性化合物开展了方法学验证。本研究建立的非靶向快速筛查无需标准品,无需复杂的方法开发,可以高通量分析数十种荧光增白剂,实现了非目标物的鉴定识别。Fluorescent whitening agents(FWAs)are a class of fluorescent dyes with whitening effects,and are widely used in textiles,paper,detergents,cosmetics,plastic toys,food contact materials and other products.In view of their harm to people and the environment,FWAs are limited by relevant regulations at home and abroad.In this work,based on high performance liquid chromatography-high resolution mass spectrometry technique,a method was established for non-targeted screening and identification of 31 kinds of FWAs,which belonged to 7 different classes,in children′s masks.And the method was successfully applied to the analysis of real masks samples from 18 different brands.Using methanol∶water(3∶1,V/V)solution as extraction solvent,the FWAs in children′s masks were extracted by ultrasonic assisted extraction.For chromatographic separation,5 mmol/L ammonium acetate and methanol were used as the mobile phase and the gradient elution was optimized.A Full mass scan and data-dependent MS/MS mode(Full MS/dd-MS 2)was used for high-resolution mass spectrometry detection.Qualitative confirmation of compounds was based on multi-dimensional information,such as exact mass,parent ion isotope abundance ratio,predicted retention time and predicted fragment ion.The fragment structures of 4 kinds of FWAs detected in children′s masks were firstly deduced by Xcalibur,Mass Frontier and ACD/MS Fragmenter software,and then compared with literature reports.Finally,the accurate qualitative and quantitative analyses were carried out by the reference standard materials of FWAs,and the methodological verification of the non-targeting method was carried out by using representative compounds.The established non-target screening method could achieve rapid analysis of FWAs with high throughput,without purchasing all reference standards and complicated method development.The method could satisfy both the regulations requirements and identification of non-target compounds.Especially during the epidemic period,it could provide an effective techni

关 键 词：高效液相色谱-高分辨质谱 荧光增白剂 儿童口罩 非靶向筛查 

分 类 号：O657.63[理学—分析化学] TS941.724[理学—化学]