Desmet Judith, Aretaki Maria A, Viana Mar, Eljarrat Ethel
Institute of Environmental Assessment and Water Research, (IDAEA)-CSIC, Jordi Girona 18-26, 08034, Barcelona, Spain.
Pollution Prevention Unit, Ministry for Ecological Transition, Pza. San Juan de La Cruz 10, 28071, Madrid, Spain.
Anal Bioanal Chem. 2025 Sep 2. doi: 10.1007/s00216-025-06057-x.
This study presents a methodology for sampling, preserving, and analyzing 15 organophosphate esters (OPEs), 11 phthalate esters (PEs), and 6 alternative plasticizers (APs) in indoor air. Accurate quantification is essential, given their widespread use in household items and adverse health effects associated with exposure. Solid-phase extraction (SPE) cartridges, collecting both gaseous and particulate phases, connected to a low-volume pump were used for the collection of air samples. Stability tests confirm that storing samples at 4 °C is most optimal to maintain analyte integrity for at least 2 weeks. The analytes were extracted and then purified online using turbulent flow chromatography, before analysis via liquid chromatography-tandem mass spectrometry (TFC-LC-MS/MS). Quantification was carried out by applying the isotopic dilution method with labelled standards. Recoveries ranged from 50 to 136%, with reproducibility below 21%. The relative standard deviation (RSD) varied from 2 to 31%, only exceeding the 20% threshold for certain OPEs at lower concentrations. Limits of detection (mLODs) varied between 0.02-0.89 ng/m, 0.02-20.0 ng/m, and 0.07-1.47 ng/m for OPEs, PEs, and APs, respectively. The study demonstrates that this methodology is effective, cost-efficient, and suitable for monitoring a total of 33 flame retardants and plasticizers in indoor air. It minimizes material costs and sample handling time by allowing direct analysis without pretreatment. Results from indoor air samples collected in a case study revealed that OPEs attributed to less than 20% of the chemical profile, while triethyl citrate (TEC) was detected at concentrations up to 28.9 ng/m, confirming the method's applicability for the added APs.
本研究提出了一种用于对室内空气中15种有机磷酸酯（OPEs）、11种邻苯二甲酸酯（PEs）和6种替代增塑剂（APs）进行采样、保存及分析的方法。鉴于它们在家庭用品中的广泛使用以及与接触相关的不良健康影响，准确的定量分析至关重要。连接到低流量泵的固相萃取（SPE）小柱用于采集空气样品，该小柱可同时收集气态和颗粒态物质。稳定性测试证实，将样品储存在4℃最有利于至少在2周内保持分析物的完整性。在通过液相色谱-串联质谱法（TFC-LC-MS/MS）分析之前，先对分析物进行萃取，然后使用湍流色谱法进行在线净化。采用标记标准品的同位素稀释法进行定量。回收率在50%至136%之间，重现性低于21%。相对标准偏差（RSD）在2%至31%之间变化，仅在较低浓度下某些OPEs超过了20%的阈值。OPEs、PEs和APs的检测限（mLODs）分别在0.02 - 0.89 ng/m、0.02 - 20.0 ng/m和0.07 - 1.47 ng/m之间。该研究表明，这种方法有效、具有成本效益，适用于监测室内空气中总共33种阻燃剂和增塑剂。它通过无需预处理即可直接分析，最大限度地降低了材料成本和样品处理时间。在一个案例研究中采集的室内空气样品结果显示，OPEs在化学组成中所占比例不到20%，而柠檬酸三乙酯（TEC）的检测浓度高达28.9 ng/m，证实了该方法对添加的APs的适用性。
