Crown ethers as shift reagents in peptide epimer differentiation –conclusions from examination of ac-(H)FRW-NH2 petide sequences

Crown ethers with different ring sizes and substituents (18-crown-6, dibenzo-18-crown-6, dicyclohexano-18-crown-6, a chiral tetracarboxylic acid-18-crown-6 ether, dibenzo-21-crown-7, and dibenzo-30-crown-10) were evaluated as shift reagents to differentiate epimeric model peptides (tri-and tetrapeptides) using ion mobility mass spectrometry (IM-MS). The stable associates of peptide epimers with crown ethers were detected and examined using traveling-wave ion mobility time-of-flight mass spectrometer (Synapt G2-S HDMS) equipped with an electrospray ion source. The overall decrease of the epimer separation upon crown ether complexation was observed. The increase of the effectiveness of the microsolvation of a basic moiety - guanidine or ammonium group in the peptide had no or little effect on the epimer discrimination. Any increase of the epimer separation, which referred to the specific association mode between crown substituents and a given peptide sequence, was drastically reduced for the longer peptide sequence (tetrapeptide). The obtained results suggest that the application of the crown ethers as shift reagents in ion mobility mass spectrometry is limited to the formation of complexes differing in stoichiometry rather than it refers to a specific coordination mode between a crown ether and a peptide molecule.

Determination of ethylene by field asymmetric ion mobility spectrometry

The determination of ethylene with a field asymmetric ion mobility spectrometer, which can easily be constructed in-house, is described. The device makes use of a Krypton lamp for ionization. A rectangular pulse of 500 Vpp at 1 MHz was employed as separation waveform in the drift tube rather than the commonly used less efficient bisinusoidal waveform. The calibration curve for the range from 670 ppb(V/V) to 67 ppm(V/V) was found to be highly linear with a correlation coefficient of r = 0.9999. The limit of detection was determined as 200 ppb(V/V). The reproducibility was 4% (relative standard deviation). The device was found to be suitable for the determination of ethylene given off by fruit; 6 types of climacteric fruit were tested, namely apples, bananas, kiwi fruit, nectarines, pears and plums.

Recovery characteristics of different tube materials in relation to combustion products

Common challenge in gas analyzers such as Ion Mobility Spectrometers (IMS) integrated into a measurement system is the reduced analysis speed that is partially limited by the temporal carry-over of sample molecules. It is caused by adsorption and absorption of the molecules into the gas tubes of the analyzer. We studied the recovery times of common tube materials: polyether ether ketone (PEEK), polytetrafluoroethylene (PTFE), fluorinated ethylene propylene (FEP), polyethylene (PE), steel 316 L, parylene C coated steel and Silconert® coated steel from organic combustion products. The tests were performed in two temperatures, at 25 °C and at 70 °C. In addition, detailed analysis was performed for PTFE tube material at 33, 50, 70 and 100 °C to observe the temperature relation of desorption. Uncoated steel was found to have the best performance in increased temperature applications due lack of absorption. Major advantages from coatings compared to plane steel were not found. Plastics were found suitable materials in lower temperatures where adsorption exceeds absorption.

Novel ion drift tube for high-performance ion mobility spectrometers based on a composite material

Ion mobility spectrometers (IMS) are able to detect pptV-level concentrations of substances in gasses and in liquids within seconds. Due to the continuous increase in analytical performance and reduction of the instrument size, IMS are established nowadays in a variety of analytical field applications. In order to reduce the manufacturing effort and further enhance their widespread use, we have developed a simple manufacturing process for drift tubes based on a composite material. This composite material consists of alternating layers of metal sheets and insulator material, which are connected to each other in a mechanically stable and gastight manner. Furthermore, this approach allows the production of ion drift tubes in just a few steps from a single piece of material, thus reducing the manufacturing costs and efforts. Here, a drift tube ion mobility spectrometer based on such a composite material is presented. Although its outer dimensions are just 15 mm × 15 mm in cross section and 57 mm in length, it has high resolving power of Rp = 62 and detection limits in the pptV-range, demonstrated for ethanol and 1,2,3-trichloropropane.