Key Laboratory for Applied Technology of Sophisticated Analytical Instruments of Shandong Province, Analysis and Test Center, Shandong Academy of Sciences, Jinan, China.
Anal Bioanal Chem. 2011 May;400(4):1189-95. doi: 10.1007/s00216-011-4857-y. Epub 2011 Mar 16.
In this paper, a simple and cheap method for the simultaneous preconcentration and sensitive determination of three hexabromocyclododecane (HBCD) diastereomers (α-, β-, and γ-HBCD) in environmental water samples has been developed. It was based on solid phase extraction (SPE) and rapid resolution liquid chromatography-electrospray tandem mass spectrometry. Bamboo charcoal, one kind of cheap material, was investigated and used as SPE adsorbent for the enrichment and determination of HBCD diastereomers. Related important parameters affecting extraction efficiencies, including type and volume of eluant, amount of sorbent, sample pH, flow rate, and sample volume, were investigated and optimized in detail. Under the optimum conditions, experimental data exhibited excellent linear relationships between peak area and concentrations over the range 0.1-10 μg L(-1). The limits of detection and precision were in the range of 0.005-0.015 μg L(-1) and 4.59-7.47%, respectively. The proposed method has been successfully applied for the trace analysis of HBCD diastereomers in real-world environmental water samples.
本文提出了一种简单、廉价的方法，用于同时浓缩和灵敏测定环境水样中的三种六溴环十二烷（HBCD）非对映异构体（α-、β-和γ-HBCD）。该方法基于固相萃取（SPE）和快速分辨液相色谱-电喷雾串联质谱法。研究并使用廉价材料竹炭作为 SPE 吸附剂，用于富集和测定 HBCD 非对映异构体。详细考察并优化了影响萃取效率的相关重要参数，包括洗脱剂的类型和体积、吸附剂的用量、样品 pH 值、流速和样品体积。在最佳条件下，实验数据表明，在 0.1-10μg/L 范围内，峰面积与浓度之间呈良好的线性关系。检测限和精密度的范围分别为 0.005-0.015μg/L 和 4.59-7.47%。该方法已成功应用于实际环境水样中 HBCD 非对映异构体的痕量分析。
