Niamlang Pimolpun, Supaphol Pitt, Morlock Gertrud E
Department of Materials Engineering, Faculty of Engineering, Rajamangala University of Technology Rattanakosin, 96 Mu 3 Phutthamonthon Sai 5 Road, Salaya, Phutthamonthon, Nakorn Pathom 73170, Thailand.
Institute of Nutritional Science, Chair of Food Science, Justus Liebig University Giessen, Heinrich-Buff-Ring 26-32, 35392 Giessen, Germany.
Nanomaterials (Basel). 2017 Aug 10;7(8):218. doi: 10.3390/nano7080218.
Research in the miniaturization of planar chromatography led to various approaches in manufacturing ultrathin-layer chromatography (UTLC) layers of reduced thickness (<50 µm) along with smaller instrumentation, as targeted in Office Chromatography. This novel concept merges 3D print & media technologies with miniaturized planar chromatography to realize an all-in-one instrument, in which all steps of UTLC are automated and integrated in the same tiny device. In this context, the development of electrospun polyacrylonitrile (PAN) nanofiber phases was investigated as well as its performance. A nanofibrous stationary phase with fiber diameters of 150-225 nm and a thickness of ca. 25 µm was manufactured. Mixtures of water-soluble food dyes were printed on it using a modified office printer, and successfully separated to illustrate the capabilities of such UTLC media. The separation took 8 min for 30 mm and was faster (up to a factor of 2) than on particulate layers. The mean values ranging from 25 to 90 for the five food dyes were well spread over the migration distance, with an overall reproducibility of 7% (mean % over 5 different plates for 5 dyes). The individual mean plate numbers over 5 plates ranged between 8286 and 22,885 (mean of 11,722 over all 5 dyes). The single mean resolutions were between 1.7 and 6.5 (for the 5 food dyes over 5 plates), with highly satisfying reproducibilities (0.3 as mean deviation of ). Using videodensitometry, different amounts separated in parallel led to reliable linear calibrations for each dye ( of 3.1-9.1% for peak heights and 2.4-9.3% for peak areas). Coupling to mass spectrometry via an elution head-based interface was successfully demonstrated for such ultrathin layers, showing several advantages such as a reduced cleaning process and a minimum zone distance. All these results underline the potential of electrospun nanofibrous phases to succeed as affordable stationary phase for quantitative UTLC.
平面色谱小型化的研究催生了多种方法,用于制造厚度更小(<50 µm)的超薄层色谱(UTLC)板,并配备更小的仪器,这也是办公色谱的目标所在。这一新颖概念将3D打印和介质技术与小型化平面色谱相结合,以实现一体化仪器,其中UTLC的所有步骤均实现自动化,并集成在同一微小设备中。在此背景下,对静电纺聚丙烯腈(PAN)纳米纤维固定相的开发及其性能进行了研究。制备了纤维直径为150 - 225 nm、厚度约为25 µm的纳米纤维固定相。使用改良的办公打印机将水溶性食用色素混合物打印在该固定相上,并成功实现分离,以展示此类UTLC介质的性能。30 mm的分离过程耗时8分钟,比颗粒板更快(快达2倍)。五种食用色素的平均值在25至90之间,在迁移距离上分布良好,总体重现性为7%(5种染料在5个不同板上的平均百分比)。5个板上各染料的平均塔板数在8286至22885之间(5种染料的平均值为11722)。单个平均分离度在1.7至6.5之间(5种食用色素在5个板上),重现性非常令人满意(平均偏差为0.3)。使用视频光密度法,平行分离的不同量可实现每种染料可靠的线性校准(峰高的相对标准偏差为3.1 - 9.1%,峰面积的相对标准偏差为2.4 - 9.3%)。通过基于洗脱头的接口与质谱联用,已成功证明此类超薄层具有多种优势,如减少清洗过程和最小化区带距离。所有这些结果都凸显了静电纺纳米纤维固定相作为定量UTLC经济适用固定相取得成功的潜力。