色谱

色谱 ›› 2017, Vol. 35 ›› Issue (10): 1080-1085.DOI: 10.3724/SP.J.1123.2017.06026

• 研究论文 • 上一篇    下一篇

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

李岩1,2, 王龙星2, 朱秀华1, 高媛2, 陈吉平2   

  1. 1. 大连交通大学环境与化学工程学院, 辽宁 大连 116028;
    2. 中国科学院大连化学物理研究所, 辽宁 大连 116023
  • 收稿日期:2017-06-27 出版日期:2017-10-08 发布日期:2017-10-18
  • 通讯作者: 朱秀华,Tel:(0411)84109335,E-mail:dlzhuxiuhua@sina.com;陈吉平,Tel:(0411)84379562,E-mail:chenjp@dicp.ac.cn.
  • 基金资助:

    国家自然科学基金项目（21577009）.

Determination of hexabromocyclododecanes in ambient air by high performance liquid chromatography- electrospray ionization-mass spectrometry

LI Yan1,2, WANG Longxing2, ZHU Xiuhua1, GAO Yuan2, CHEN Jiping2   

  1. 1. School of Environmental and Chemical Engineering, Dalian Jiaotong University, Dalian 116028, China;
    2. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China
  • Received:2017-06-27 Online:2017-10-08 Published:2017-10-18
  • Supported by:

    Foundation item:National Natural Science Foundation of China (No. 21577009).

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摘要：

优化了环境大气样品前处理步骤中复合硅胶柱的净化条件，建立了高效液相色谱-电喷雾-质谱（HPLC-ESI-MS）测定环境大气中六溴环十二烷（hexabromocyclododecanes， HBCDs）的分析方法。样品经正己烷提取后，采用复合硅胶柱净化，以50 mL正己烷和100 mL正己烷-二氯甲烷（9 ∶ 1， v/v）为淋洗液，以180 mL正己烷-二氯甲烷（4 ∶ 1， v/v）为洗脱液。采用UF-ODS柱（150 mm×2.1 mm， 3.0 μm），以乙腈-甲醇-水为流动相进行梯度洗脱，在电喷雾负离子源、选择离子监测（SIM）模式下检测。在优化的条件下， α -HBCD、 β -HBCD和 γ -HBCD能很好地分离，在1~100 μg/L范围内， α -HBCD、 β -HBCD和 γ -HBCD与进样内标D18- γ -HBCD峰面积的比值与对应的质量浓度均具有良好的线性关系，相关系数（R）≥0.9988。 α -HBCD、 β -HBCD和 γ -HBCD的仪器检出限（S/N=3）分别为0.4、0.5和0.4 μg/L；定量限（S/N=10）分别为1.4、1.6和1.3 μg/L；方法检出限（MDL）分别为0.13、0.17和0.13 pg/m3 （n=5）；实际样品的加标回收率为74.8%~95.8%。该法灵敏度高，选择性好，可以满足大气样品中HBCDs的监测和分析需求。

关键词: 大气, 高效液相色谱-电喷雾-质谱, 六溴环十二烷

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 monitoring (SIM) mode were adopted in MS detection. The results showed that α -HBCD, β -HBCD and γ -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 relationship, 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 demonstrated that the method has high sensitivity and good selectivity, and can meet the requirement of monitoring and analyzing HBCDs in air samples.

Key words: air, hexabromocyclododecanes (HBCDs), high performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS)

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