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Stir bar sorptive extraction and thermal desorption – gas chromatography/mass spectrometry for determining phosphorus flame retardants in air samples†
Analytical Methods ( IF 3.1 ) Pub Date : 2018-03-22 00:00:00 , DOI: 10.1039/c8ay00138c
Julius Matsiko 1, 2, 3, 4, 5 , Honghua Li 1, 2, 3, 4, 5 , Pu Wang 1, 2, 3, 4, 5 , Huizhong Sun 1, 2, 3, 4, 5 , Shucheng Zheng 1, 2, 3, 4, 5 , Dou Wang 1, 2, 3, 4, 5 , Weiwei Zhang 1, 2, 3, 4, 5 , Yanfen Hao 1, 2, 3, 4, 5 , Yingming Li 1, 2, 3, 4, 5 , Qinghua Zhang 1, 2, 3, 4, 5 , Guibin Jiang 1, 2, 3, 4, 5
Affiliation  

Stir bar sorptive extraction and thermal desorption coupled with gas chromatography/mass spectrometry (SBSE-TD-GC/MS) was utilized to determine phosphorus flame retardants (PFRs) in air samples. The one variable at a time (OVAT) approach was used to select the optimal conditions of the parameters that affect the SBSE procedure during thermal desorption. Desorption was carried out at 300 °C at a desorption flow rate of 76 mL min−1 for 10 minutes with the transfer line set at 320 °C. The analytes were cryofocused at −40 °C and then cryo-desorbed at 320 °C for 2 minutes. The optimal desorption conditions were then used to validate the method. The method validation showed good linearity (r2 > 0.9960), good precision (CVs ≤ 20%), low limits of detection (8.7–14.0 pg), good recoveries (>70%) and high reliability. Passive air sampling based on polydimethylsiloxane (PDMS) coated stir bars together with high volume-active air sampling (HV-AAS) (for comparison and calibration) was used to ascertain the appropriateness of the proposed method to determine the concentrations of PFRs in real air samples. The concentration results obtained by the two sampling techniques were comparable for compounds, whose passive samplers' accumulated masses were above the limits of quantitation and showed good uptake linearity over a specific period of time during the deployment. This work therefore affirms that the proposed method performs well and thus can be a suitable and cheaper alternative to active air sampling for gas phase PFRs.

中文翻译:

搅拌棒吸附萃取和热脱附–气相色谱/质谱法测定空气样品中的磷阻燃剂

搅拌棒吸附萃取和热脱附结合气相色谱/质谱法(SBSE-TD-GC / MS)用于测定空气样品中的磷阻燃剂(PFR)。一次使用一个变量(OVAT)方法来选择影响热脱附过程中SBSE程序的参数的最佳条件。在传输线设定为320℃的条件下,在300℃下以76mLmin -1的解吸流速进行10分钟的解吸。将分析物在-40°C低温聚焦,然后在320°C低温解吸2分钟。然后使用最佳解吸条件对方法进行验证。方法验证显示出良好的线性(r 2> 0.9960),良好的精度(CV≤20%),低检测限(8.7–14.0 pg),良好的回收率(> 70%)和高可靠性。基于聚二甲基硅氧烷(PDMS)涂覆的搅拌棒的被动空气采样以及高容量主动空气采样(HV-AAS)(用于比较和校准)被用来确定所提出的确定真实空气中PFR浓度的方法的适当性样品。通过两种采样技术获得的浓度结果与化合物相当,其被动采样器的累积质量超过了定量极限,并且在展开过程中的特定时间段内显示出良好的吸收线性。因此,这项工作肯定了所提出的方法性能良好,因此可以作为气相PFR主动空气采样的一种合适且便宜的替代方法。
更新日期:2018-03-22
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