The analysis of volatile organic compounds (VOCs) normally involves sample collection, sample transfer to laboratory, sample preparation, and the chromatographic separation of analytes. However, in some cases, it is impractical or impossible to collect samples prior to the analysis, while the analysis time has to be minimized. Ion mobility spectrometry (IMS) is an ideal technique for a rapid in situ chemical analysis. Here, we present a portable cloud-integrated pen-probe analyzer based on IMS and demonstrate its applications in the analysis of VOCs emanating from surfaces. The user approaches the penprobe to a sampled surface and presses a button on the pen-probe. The analysis is then executed automatically. The VOCs are scavenged from the surface by a suction force and directed to a corona discharge atmospheric pressure chemical ionization source. The ions are separated in a drift tube according to their size and charge and then detected by a Faraday plate detector. The detector signal is amplified and digitized. The spectral data are deposited in the Internet cloud along with time and location data for further retrieval and processing. The platform incorporates a mobile Wi-Fi router for easy connectivity and a global positioning system module for geolocation. The prototype was developed using low-cost electronic modules (Arduino, Tinker Board S). It was further characterized using chemical standards. The limits of detection for pyrrolidine, 2,4-lutidine, and (−)-nicotine are 48.9, 2.30, and 416 nmol, respectively (amounts of substances placed on the sampling surface). The selected real specimens (nicotine patch, skin exposed to nicotine, fish sauce, and fried chicken) were also subjected to analysis yielding the characteristic ion mobility spectra.
Sparging-based methods have long been used to liberate volatile organic compounds (VOCs) from liquid sample matrices prior to analysis. In these methods, a carrier gas is delivered from an external source. Here, we demonstrate “catalytic oxygenation-mediated extraction” (COME), which relies on biocatalytic production of oxygen occurring directly in the sample matrix. The newly formed oxygen (micro)bubbles extract the dissolved VOCs. The gaseous extract is immediately transferred to a separation or detection system for analysis. To start COME, dilute hydrogen peroxide is injected into the sample supplemented with catalase enzyme. The entire procedure is performed automaticallyafter pressing a “start” button, making a clapping sound, or triggering from a smartphone. The pump, valves, and detection system are controlled by a microcontroller board. For quality control and safety purposes, the reaction chamber is monitored by a camera linked to a single-board computer, which follows the enzymatic reaction progress by analyzing images of foam in real time. The data are instantly uploaded to the internet cloud for retrieval. The COME apparatus has been coupled on-line with the gas chromatography electron ionization mass spectrometry (MS) system, atmospheric pressure chemical ionization (APCI) MS system, and APCI ion-mobility spectrometry system. The three hyphenated variants have been tested in analyses of complex matrices (e.g., fruit-based drinks, whiskey, urine, and stored wastewater). In addition to the use of catalase, COME variants using crude potato pulp or manganese(IV) dioxide have been demonstrated. The technique is inexpensive, fast, reliable, and green: it uses low-toxicity chemicals and emits oxygen.
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