Chen Yu-Hsuan, Chang Chia-Yu, Ding Wang-Hsien
Department of Chemistry, National Central University, Chung-Li 320, Taiwan.
Department of Chemistry, National Central University, Chung-Li 320, Taiwan.
J Chromatogr A. 2016 Nov 11;1472:129-133. doi: 10.1016/j.chroma.2016.10.048. Epub 2016 Oct 19.
A simple and effective method for determining short chain chlorinated paraffins (SCCPs) in indoor dust is presented. The method employed a modified vortex-homogenized matrix solid-phase dispersion (VH-MSPD) prior to its detection by gas chromatography - electron-capture negative-ion mass spectrometry (GC-ECNI-MS) operating in the selected-ion-monitoring (SIM) mode. Under the best extraction conditions, 0.1-g of dust sample was dispersed with 0.1-g of silica gel by using vortex (2min) instead of using a mortar and pestle (3min). After that step, the blend was transferred to a glass column containing 3-g acidic silica gel, 2-g basic silica gel, and 2-g of deactivated silica gel, used as clean-up co-sorbents. Then, target analytes were eluted with 5mL of n-hexane/dichloromethane (2:1, v/v) mixture. The extract was evaporated to dryness under a gentle stream of nitrogen. The residue was then re-dissolved in n-hexane (10μL), and subjected to GC-ECNI-MS analysis. The limits of quantitation (LOQs) ranged from 0.06 to 0.25μg/g for each SCCP congener. Precision was less than 7% for both intra- and inter-day analysis. Trueness was above 89%, which was calculated by mean extraction recovery. The VH-MSPD combined with GC-ECNI-MS was successfully applied to quantitatively detect SCCPs from various indoor dust samples, and the concentrations ranged from 1.2 to 31.2μg/g.
本文介绍了一种简单有效的测定室内灰尘中短链氯化石蜡（SCCPs）的方法。该方法在采用气相色谱-电子捕获负离子质谱（GC-ECNI-MS）以选择离子监测（SIM）模式进行检测之前，先采用了改进的涡旋均质化基质固相分散（VH-MSPD）方法。在最佳提取条件下，用0.1 g硅胶通过涡旋（2分钟）而非研钵和杵研磨（3分钟）来分散0.1 g灰尘样品。此步骤之后，将混合物转移至装有3 g酸性硅胶、2 g碱性硅胶和2 g失活硅胶的玻璃柱中，这些硅胶用作净化共吸附剂。然后，用5 mL正己烷/二氯甲烷（2:1，v/v）混合物洗脱目标分析物。提取物在温和的氮气流下蒸发至干。残渣随后用正己烷（10μL）重新溶解，并进行GC-ECNI-MS分析。每种SCCP同系物的定量限（LOQs）范围为0.06至0.25μg/g。日内和日间分析的精密度均小于7%。通过平均提取回收率计算得出的准确度高于89%。VH-MSPD与GC-ECNI-MS相结合成功应用于定量检测各种室内灰尘样品中的SCCPs，其浓度范围为1.2至31.2μg/g。
