RESUMO
Online monitoring of exhaled propofol concentration is important for anesthetists to provide adequate anesthesia as propofol concentrations in plasma and breath are correlated reasonably well. Exhaled propofol could be detected by 63Ni ion mobility spectrometry in negative ion mode; however, the radioactivity of 63Ni source restricts its clinical application due to safety, environmental, and regulatory concerns. An acetone-assisted negative photoionization ion mobility spectrometer (AANP-IMS) using a side-mounted vacuum ultraviolet (VUV) lamp in the unidirectional (UD) flow mode was developed for sensitive measurement of exhaled propofol by producing a high percentage of O2-(H2O) n. An adsorption sampling and time-resolved purge introduction system was developed to eliminate the interference of residual inhaled anesthetic sevoflurane based on their different adsorptions between propofol and sevoflurane on the inwall of the fluorinated ethylene propylene (FEP) sample loop. The effects of the inner diameter and the length of the sample loop on the signal intensity of propofol and the time-resolution between propofol and sevoflurane were theoretically and experimentally investigated. A sample loop with 3 mm i.d. and 150 cm length allowed sensitive measurement of exhaled propofol with a response time of 4 s, a linear response range for propofol was achieved to be 0.2 to 14 ppbv with a limit of detection (LOD) of 60 pptv, and the quantification of propofol was not influenced by the change of the sevoflurane concentration. Finally, the performance of monitoring exhaled propofol during surgery was demonstrated on a patient undergoing laparoscopic distal pancreatectomy combined with cholecystectomy.
Assuntos
Acetona/química , Expiração , Monitorização Intraoperatória , Sistemas On-Line , Propofol/análise , Testes Respiratórios , Humanos , Espectrometria de Mobilidade Iônica , Fatores de TempoRESUMO
With respect to massive consumption of ammonia and rigorous industrial synthesis conditions, many studies have been devoted to investigating more environmentally benign catalysts for ammonia synthesis under moderate conditions. However, traditional methods for analysis of synthesized ammonia (e.g., off-line ion chromatography (IC) and chemical titration) suffer from poor sensitivity, low time resolution, and sample manipulations. In this work, charge-transfer ionization (CTI) with O2(+) as the reagent ion based on a vacuum ultraviolet (VUV) lamp in a time-of-flight mass spectrometer (CTI-TOFMS) has been applied for real-time monitoring of the ammonia synthesis in a microreactor. For the necessity of long-term stable monitoring, a self-adjustment algorithm for stabilizing O2(+) ion intensity was developed to automatically compensate the attenuation of the O2(+) ion yield in the ion source as a result of the oxidation of the photoelectric electrode and contamination on the MgF2 window of the VUV lamp. A wide linear calibration curve in the concentration range of 0.2-1000 ppmv with a correlation coefficient (R(2)) of 0.9986 was achieved, and the limit of quantification (LOQ) for NH3 was in ppbv. Microcatalytic synthesis of ammonia with three catalysts prepared by transition-metal/carbon nanotubes was tested, and the rapid changes of NH3 conversion rates with the reaction temperatures were quantitatively measured with a time resolution of 30 s. The high-time-resolution CTI-TOFMS could not only achieve the equilibrium conversion rates of NH3 rapidly but also monitor the activity variations with respect to investigated catalysts during ammonia synthesis reactions.
RESUMO
A nano-electrospray ionization-ion mobility spectrometer (nanoESI-IMS) was built up. Firstly, the effects of the parameters such as drift gas flow rate and solvent flow rate on the desolvation capability were studied and optimized. Then, a series of compounds were used to characterize the nanoESI-IMS system. The results showed that, complete desolvation was achieved for nano-electrospray ion droplets with the nanoESI-IMS apparatus. The limit of detection of this instrument for trioctylamine could reach 10 microg/L. Finally, this instrument was coupled to the high performance liquid chromatography (HPLC) as a detector for amines analysis. A test mixture containing triethylamine, diethylamine and butylamine was successfully separated and determined by the HPLC-nanoESI-IMS system. Linear response ranges of about two orders of magnitude were achieved for triethylamine, diethylamine and butylamine with this system.
RESUMO
An ion mobility spectrometer array was designed, in order to broaden the detection range of ion mobility spectrometer and improve the accuracy of compound identification. This instrument was based on the combination of ionization sources of 63Ni positive ion mode, 63Ni negative ion mode and photoionization mode with vacuum UV lamp, and it can continuously monitor the volatile organic compounds in air. With the automatic system of sampling and injection of this instrument, the positive ion of dimethyl sulfoxide and negative ion of dichloromethane were detected simultaneously. By comprehensive analysis of spectra with ion mobility spectrometer array, acrylonitrile, m-xylene and acetone were identified, which were difficult to be distinguished under the 63Ni positive ion mode. Acetone samples were determined quantitatively within four days continuously, and the results indicated that the linear range of acetone in this instrument was 2 orders of magnitude. The linear correlation coefficient R was higher than 0.995, and the relative standard deviations were controlled in the range of 4.0%-18.3%. Methacrylate leaked in simulation was monitored on-line for 24 h continuously, using the method of dynamic tracking, and the result showed the leaking time and the concentration of methacrylate directly.