Use of Rapid Reduced Electric Field Switching to Enhance Compound Specificity for Proton Transfer Reaction-Mass Spectrometry.
The high sensitivity of proton transfer reaction-mass spectrometry (PTR-MS) makes it a suitable analytical tool for detecting trace compounds. Its specificity is primarily determined by the accuracy of identifying the m/ z of the product ions specific to a particular compound. However, specificity can be enhanced by changing the product ions (concentrations and types) through modifying the reduced electric field. For current PTR-MS systems, this is not possible for trace compounds that would only be present in the reaction chamber of a PTR-MS for a short time (seconds). For such circumstances, it is necessary to change the reduce electric field swiftly if specificity enhancements are to be achieved. In this paper we demonstrate such a novel approach, which permits any compound that may only be present in the drift tube for seconds to be thoroughly investigated. Specifically, we have developed hardware and software which permits the reaction region's voltages to be rapidly switched at a frequency of 0.1-5 Hz. We show how this technique can be used to provide a higher confidence in the identification of compounds than is possible by keeping to one reduced electric field value through illustrating the detection of explosives. Although demonstrated for homeland security applications, this new technique has applications in other analytical areas and disciplines where rapid changes in a compound's concentration can occur, for example, in the Earth's atmosphere, plant emissions and in breath. Importantly, this adaptation provides a method for improved selectivity without expensive instrumental changes or the need for high mass resolution instruments.
Ammonia-Assisted Proton Transfer Reaction Mass Spectrometry for Detecting Triacetone Triperoxide (TATP) Explosive
AbstractProton transfer reaction mass spectrometry (PTR-MS) usually detects different types of compounds by changing the discharge gas to produce different reagent ions in the ion source. In the present work, a novel method of changing reagent ions, ammonia-assisted PTR-MS, was developed. Through an injection port bypass, ammonia was injected into a homemade PTR-MS device. A conventional PTR-MS apparatus with reagent ions H3O+(H2O)n (n = 0, 1, 2) can be converted to an ammonia-assisted PTR-MS with reagent ions NH4+.The new method was introduced to detect triacetone triperoxide (TATP) explosive material. Results showed that the sensitivity is enhanced more than 37 times compared with TATP detection using conventional PTR-MS and the limit of detection (LOD) could reach 1.3 ppb. TATP in real complex matrixes can also be detected successfully using this method. Compared to conventional PTR-MS, ammonia-assisted PTR-MS has better sensitivity and better LOD for TATP detection, and the technique provides common users with a convenient and quick method to change reagent ions. The users of PTR-MS can easily obtain other reagent ions by injecting different assisted gases into an injection port to meet different detection needs.
 Graphical Abstract
HPLC determination of chlorhexidine gluconate and p-chloroaniline in topical ointment.
A novel fast isocratic reversed-phase HPLC method for simultaneous determination of chlorhexidine and its degradation product p-chloroaniline was developed. Zorbax SB Phenyl column (75 mm x 4.6 mm, 3.5 microm) was used for the separation. Mobile phase composed of acetonitrile and buffer solution of 0.08 M sodium phosphate monobasic containing 5 ml of triethylamine (0.5%) and adjust with 85% phosphoric acid to pH 3.0 in ratio 35:65 (v/v) pumped isocratically at flow rate 0.6 ml min(-1) was used. UV detection was performed at 239 nm, the total analysis time was about 10 min. The method is suitable for practical routine analysis of topical ointment in the quality control laboratory.