摘要
确证江苏省重点地区环境空气样品中的一种未知醛酮类化合物.根据我国环境行业标准《环境空气醛酮类化合物的测定高效液相色谱法》(HJ 683—2014),采用高效液相色谱-二极管阵列检测法(HPLC-PDA),通过对实际环境空气样品和标准溶液的保留时间和紫外光谱图比对发现,江苏省重点地区环境空气样品中普遍存在一种醛酮类未知化合物.利用高效液相色谱-四极杆/飞行时间高分辨质谱(HPLC-QTOF-HRMS)采集正离子模式下的色谱图,获取未知化合物的精确质量数、同位素分布信息和二级质谱碎片信息,利用SCIEX OS软件对数据进行解析,推测该化合物衍生化前分子式为C_(9)H_(10)O.根据分子式推测可能的结构式,购买相关纯品,结合二级质谱碎片信息、色谱保留时间和紫外光谱图等,综合确证假阳性化合物为3,4-二甲基苯甲醛.本研究可为实际环境样品中未知化合物的筛查和结构确证提供可借鉴的思路.
In this study,an unknown aldehyde and ketone compound has been confirmed in ambient air samples collected from key areas in Jiangsu Province.According to environmental protection standard of China“Determination of aldehyde and ketone compounds-High performance liquid chromatography in ambient air samples”(HJ 683-2014),a high-performance liquid chromatography coupled with diode array detection(HPLC-PDA)technique was used.By comparing the retention time and UV absorption spectrum,a aldehyde and ketone compound has been prevailingly detected in ambient air samples.In addition,high-performance liquid chromatography–quadrupole time-offlight high resolution MS(HPLC-QTOF-HRMS)was used to collect chromatograms under positive ion mode.The accurate mass,isotope distribution,and secondary mass fragmentation information of the unknown compound were obtained.These data were further analyzed by SCIEX OS software,and the molecular formula prior to derivatization was proposed as C_(9)H_(10)O.Referring to the information of the molecular formula,authentic standard,secondary fragments spectral configuration,retention time,and UV spectrum,the false positive compound was comprehensively confirmed as 3,4-dimethylbenzaldehyde.In this paper,the structure of a false positive compound of aldehydes and ketones in actual samples was derived and confirmed by HPLC-PDA and HPLCQTOF-HRMS technology.The common screening and confirmation processes of unknown substances were summarized,which could provide useful information for the screening and structural confirmation of unknown compounds in the actual environmental samples.
作者
张蓓蓓
孙慧婧
陈慧敏
ZHANG Beibei;SUN Huijing;CHEN Huimin(State Environmental Protection Key Laboratory of Monitoring and Analysis for Organic Pollutants in Surface Water,Environment Monitoring Center of Jiangsu Province,Nanjing,210019,China;Shanghai AB Sciex Analytical Instrument Trading Co,Ltd,Shanghai,200335,China)
出处
《环境化学》
CAS
CSCD
北大核心
2023年第5期1604-1611,共8页
Environmental Chemistry
基金
江苏省环境监测科研基金(1909)资助.
关键词
醛酮类
未知化合物
结构确证
环境空气
江苏省
aldehydes and ketones
unknown compound
structural confirmation
ambient air
Jiangsu Province
