Oak Ridge Institute for Science and Education (ORISE), USEPA, Cincinnati, OH, 45220, USA.
Center for Environmental Solutions and Emergency Response, Office of Research and Development, United States Environmental Protection Agency, 26 West Martin Luther King Dr., Cincinnati, OH, 45268, USA.
Anal Bioanal Chem. 2022 Dec;414(29-30):8353-8364. doi: 10.1007/s00216-022-04371-2. Epub 2022 Oct 25.
A high-throughput approach to detecting, quantifying, and characterizing microplastics (MPs) by shape, size, and polymer type using laser direct infrared (LDIR) spectroscopy in surface water samples is demonstrated. Three urban creeks were sampled for their MP content near Cincinnati, OH. A simple Fenton reaction was used to oxidize the surface water samples, and the water samples were filtered onto a gold-coated polyester membrane. Infrared (IR) analysis for polymer identification was conducted, with recoveries of 88.3% ± 1.2%. This method was able to quantify MPs down to a diameter of 20 µm, a size comparable to that of MPs quantified by other techniques such as Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy. A shape-classifying algorithm was designed using the aspect ratio values of particles to categorize MPs as fibers, fibrous fragments, fragments, spherical fragments, or spheres. Cut-off values were identified from measurements of known sphere, fragment, and fibrous particles. About half of all environmental samples were classified as fragments while the other shapes accounted for the other half. A cut-off hit quality index (HQI) value of 0.7 was used to classify known and unidentified particles based on spectral matches to a reference library. Center for Marine Debris Research Polymer Kit 1.0 standards were analyzed by LDIR and compared to the given FTIR spectra by HQI, showing that LDIR obtains similar identifications as FTIR analysis. The simplicity and automation of the LDIR allows for quick, reproducible particle analysis, making LDIR attractive for high-throughput analysis of MPs.
本研究展示了一种高通量方法,可通过激光直接红外(LDIR)光谱法,根据形状、尺寸和聚合物类型来检测、定量和表征地表水中的微塑料(MPs)。本研究在俄亥俄州辛辛那提市附近的三条城市溪流中采集了水样,以检测其 MPs 含量。采用简单的芬顿反应氧化地表水样,然后将水样过滤到镀金聚酯膜上。对聚合物进行了红外(IR)分析,回收率为 88.3%±1.2%。该方法能够定量检测到直径为 20μm 的 MPs,这一尺寸与傅里叶变换红外光谱(FTIR)和拉曼光谱等技术定量检测的 MPs 尺寸相当。设计了一种基于颗粒纵横比值的形状分类算法,将 MPs 归类为纤维、纤维状碎片、碎片、球形碎片或球体。通过对已知球体、碎片和纤维状颗粒的测量,确定了截断值。大约一半的环境样本被归类为碎片,而其他形状则占另一半。采用 HQI 值为 0.7 的截止命中质量指数(HQI),根据与参考库的光谱匹配,对已知和未知颗粒进行分类。采用 LDIR 对海洋废弃物研究中心聚合物试剂盒 1.0 标准进行了分析,并通过 HQI 与给定的 FTIR 光谱进行了比较,结果表明 LDIR 与 FTIR 分析获得了相似的识别结果。LDIR 操作简单且自动化,能够快速、可重复地进行颗粒分析,因此对于 MPs 的高通量分析具有吸引力。