色谱2017，Vol.35Issue(10)：1080-1085,6.DOI:10.3724/SP.J.1123.2017.06026
高效液相色谱-电喷雾质谱法测定环境大气中的六溴环十二烷
Determination of hexabromocyclododecanes in ambient air by high performance liquid chromatography-electrospray ionization-mass spectrometry
摘要
Abstract
A high performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS ) method was developed for the determination of hexabromocyclododecanes (HBCDs ) in ambient air samples. The samples were extracted by Soxhlet extractor with hexane,then purified on the composite gel column. At first,the interfering substances were rinsed with 50 mL hexane and 100 mL hexane-dichloromethane (9:1,v/v),then 180 mL hexane-dichloromethane (4:1,v/v)was used to elute the targets. The compounds were separated by gradient elution with acetonitrile-methanol-water as mobile phases on a UF-ODS column (150 mm×2. 1 mm,3. 0 μm). Electrospray ionization negative ion source and selective ion monito-ring (SIM)mode were adopted in MS detection. The results showed thatα-HBCD,β-HBCD andγ-HBCD could be well separated,and the chromatographic peak area ratio of α-HBCD,β-HBCD and γ-HBCD to internal standard D18-γ-HBCD with their concentrations had a good linear rela-tionship,with the correlation coefficients (R)≥0. 9988. The limits of detection (LODs,S/N=3)of α-HBCD,β-HBCD and γ-HBCD were 0. 4,0. 5 and 0. 4 μg/L,respectively. The limits of quantification (LOQs,S/N = 10 ) were 1. 4,1. 6 and 1. 3 μg/L,respectively. The method detection limits (MDL)were 0. 13,0. 17 and 0. 13 pg/m3 (n=5),respectively. The recoveries of HBCDs spiked in the actual air samples were in the range of 74. 8%-95. 8%. It is demonstra-ted that the method has high sensitivity and good selectivity,and can meet the requirement of monitoring and analyzing HBCDs in air samples.关键词
高效液相色谱-电喷雾-质谱/六溴环十二烷/大气Key words
high performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS)/hexabromocyclododecanes (HBCDs)/air分类
化学化工引用本文复制引用
李岩,王龙星,朱秀华,高媛,陈吉平..高效液相色谱-电喷雾质谱法测定环境大气中的六溴环十二烷[J].色谱,2017,35(10):1080-1085,6.基金项目
国家自然科学基金项目(21577009).National Natural Science Foundation of China (No. 21577009). （21577009）
