High-resolution atmospheric pressure infrared laser desorption/ionization mass spectrometry imaging of biological tissue.

An atmospheric pressure laser desorption/ionization mass spectrometry imaging ion source has been developed that combines high spatial resolution and high mass resolution for the in situ analysis of biological tissue. The system is based on an infrared laser system working at 2.94 to 3.10 µm wavelength, employing a Nd:YAG laser-pumped optical parametrical oscillator. A Raman-shifted Nd:YAG laser system was also tested as an alternative irradiation source. A dedicated optical setup was used to focus the laser beam, coaxially with the ion optical axis and normal to the sample surface, to a spot size of 30 µm in diameter. No additional matrix was needed for laser desorption/ionization. A cooling stage was developed to reduce evaporation of physiological cell water. Ions were formed under atmospheric pressure and transferred by an extended heated capillary into the atmospheric pressure inlet of an orbital trapping mass spectrometer. Various phospholipid compounds were detected, identified, and imaged at a pixel resolution of up to 25 µm from mouse brain tissue sections. Mass accuracies of better than 2 ppm and a mass resolution of 30,000 at m/z = 400 were achieved for these measurements.

Biodegradability screening of soil amendments through coupling of wavelength-scanned cavity ring-down spectroscopy to multiple dynamic chambers.

A system was developed for the automatic measurements of ¹³CO2 efflux to determine biodegradation of extra carbon amendments to soils. The system combines wavelength-scanned cavity ring down laser spectroscopy (WS-CRDS) with the open-dynamic chamber (ODC) method. The WS-CRDS instrument and a batch of 24 ODC are coupled via microprocessor-controlled valves. Determination of the biodegradation requires a known δ¹³C value and the applied mass of the carbon compounds, and the biodegradation is calculated based on the ¹³CO2 mixing ratio (ppm) sampled from the headspace of the chambers. The WS-CRDS system provided accurate detection based on parallel samples of three standard gases (¹³CO2 of 2, 11 and 22 ppm) that were measured simultaneously by isotope ratio mass spectrometry (linear regression R² = 0.99). Repeated checking with the same standards showed that the WS-CRDS system showed no drift over seven months.The applicability of the ODC was checked against the closed static chamber (CSC) method using the rapid biodegradation of cane sugar-δ¹³C-labeled through C4 photosynthesis. There was no significant difference between the results from 7-min ODC and 120-min CSC measurements. Further, a test using samples of either cane sugar (C4) or beetroot sugar (C3) mixed into standard soil proved the target functionality of the system, which is to identify the biodegradation of carbon sources with significantly different isotopic signatures.