Ueta Ikuo, Mochizuki Suguru, Kawakubo Susumu, Kuwabara Tetsuo, Jinno Kiyokatsu, Saito Yoshihiro
Department of Applied Chemistry, University of Yamanashi, 4-3-11 Takeda, Kofu, 400-8511, Japan.
Anal Bioanal Chem. 2015 Jan;407(3):899-905. doi: 10.1007/s00216-014-8144-6. Epub 2014 Sep 9.
A novel miniaturized sample extraction capillary was developed to provide a simple and sensitive method for analyzing gaseous formaldehyde (FA) using conventional high-performance liquid chromatography (HPLC). The extraction capillary was prepared by packing silica gel particles in a stainless steel capillary with a 1.6-mm o.d. Before the gaseous samples were collected, the silica gel particles were impregnated with a derivatizing reagent 2,4-dinitrophenylhydrazine (DNPH) by passing a solution of DNPH through the extraction capillary. FA was derivatized to form the corresponding hydrazone during the active sampling of a gaseous sample, and the derivative was sorbed by the silica gel. The capillary was then directly connected to a six-port valve, and desorption from the capillary and injection into the HPLC were achieved simultaneously by passing a solvent through the capillary. The run-to-run and device-to-device variabilities, as relative standard deviations, were both less than 6.9%. The limit of detection for FA was 2.5 ng/L using a sampling volume of 100 mL, and a sample collection time of 2 min. Acetaldehyde and acetone in a gaseous sample could also be simultaneously extracted and determined using this method. The applicability of the developed method for determining FA in real indoor air samples was confirmed by comparing the results obtained using the proposed method and a conventional sample preparation method. The developed method enables the rapid and simple sample preparation of gaseous FA and gives a good level of sensitivity.
开发了一种新型小型化样品萃取毛细管,以提供一种简单且灵敏的方法,用于使用传统高效液相色谱法(HPLC)分析气态甲醛(FA)。萃取毛细管是通过将硅胶颗粒填充到外径为1.6毫米的不锈钢毛细管中制备而成。在采集气态样品之前,通过使2,4-二硝基苯肼(DNPH)溶液通过萃取毛细管,将硅胶颗粒用衍生试剂DNPH浸渍。在气态样品的主动采样过程中,FA被衍生形成相应的腙,衍生物被硅胶吸附。然后将毛细管直接连接到六通阀,通过使溶剂通过毛细管,同时实现从毛细管的解吸和注入HPLC。作为相对标准偏差,批间和设备间的变异性均小于6.9%。使用100 mL的采样体积和2分钟的样品采集时间,FA的检测限为2.5 ng/L。气态样品中的乙醛和丙酮也可以使用该方法同时萃取和测定。通过比较使用所提出的方法和传统样品制备方法获得的结果,证实了所开发方法用于测定实际室内空气样品中FA的适用性。所开发的方法能够实现气态FA的快速简单样品制备,并具有良好的灵敏度水平。