Related Articles

• Elemental Compositions from Exact Mass Measurements and Accurate Isotopic Abundances

  Exact masses have been used for decades to calculate elemental compositions for known and unknown molecules. The traditional approach calculates all possible combinations of user-specified atoms that fall within a given error tolerance of a measured mass. The number of possible combinations increases dramatically with increasing mass and as more atoms are included in the search set. In many cases, it is not possible to determine a unique composition based on mass alone. A common source of error in measuring isotopic abundances with scanning mass spectrometers is related to fluctuations in ion current during measurement. The AccuTOF family of mass spectrometers overcomes this problem by analyzing all of the isotopes formed at the same instant. Combined with a high-dynamic-range detector, this provides highly accurate isotopic abundances. It has been shown that accurately measured isotopic abundances can be combined with measured exact masses to dramatically reduce the number of possible elemental compositions for an unknown. It is often possible to deduce a unique elemental composition, facilitating the identification of unknown substances.
• Accurate Isotope Data is Essential for Determining Elemental Compositions

  Elemental compositions are commonly determined from high-resolution mass spectra and accurate mass measurements. Given a measured mass (m/z) and a range of elements that can be present, software calculates the exact mass for each combination of elements and reports all elemental combinations that match the measured mass within a specified error tolerance. Improving the mass accuracy reduces the number of elemental compositions, but mass accuracy alone may not be sufficient to determine the correct elemental composition for an unknown sample. JEOL AccuTOF™ mass spectrometers (the AccuTOF™-DART®, the AccuTOF™-GCX and the AccuTOF™-GCX Plus) are capable of accurate isotope measurements that can be used to determine elemental compositions from high-resolution mass spectra. Matching the measured abundances and exact masses for isotope peaks can be more effective than mass accuracy alone.
• High-speed 50 Hz Data AcquisitionCapability for Comprehensive 2-dimensional GC Measurements

  The comprehensive 2-dimensional GC (GC x GC) technique provides higher-separation capabilities for complex mixtures than the typical 1-dimensional GC measurements. However, the GC x GC technique requires high speed data acquisition, e. g. > 20 Hz, for the GC detectors due to the shorter 2nd GC column which elutes samples within just a few seconds (comparable to those used for the ultra-fast GC measurements). Recently, JEOL has developed a new generation GC-HRTOFMS system called the “AccuTOF GCv 4G”. The AccuTOF GCv 4G has high sensitivity, high resolution, high mass accuracy and high speed data acquisition, all simultaneously. In fact, this instrument can measure data using up to a 50 Hz data acquisition speed which is more than sufficient to do not only fast GC measurements but also GC x GC measurements.
• Ionization Methods in Organic Mass Spectrometry

  A mass spectrometer works by using magnetic and electric fields to exert forces on charged particles (ions) in a vacuum. Therefore, a compound must be charged or ionized to be analyzed by a mass spectrometer. Furthermore, the ions must be introduced in the gas phase into the vacuum system of the mass spectrometer. This is easily done for gaseous or heat-volatile samples. However, many (thermally labile) analytes decompose upon heating. These kinds of samples require either desorption or desolvation methods if they are to be analyzed by mass spectrometry. Although ionization and desorption/desolvation are usually separate processes, the term "ionization method" is commonly used to refer to both ionization and desorption (or desolvation) methods. The choice of ionization method depends on the nature of the sample and the type of information required from the analysis. So-called 'soft ionization' methods such as field desorption and electrospray ionization tend to produce mass spectra with little or no fragment-ion content.
• GCxGC-EI and GCxGC-FI Measurements Using the EI-FI Combination Ion Source

  Comprehensive 2-dimensional GC (GC x GC) provides higher-separation capabilities for complex mixtures than the typical 1-dimensional GC measurements. However, this technique requires high speed data acquisition, e. g. > 20 Hz, for the GC detectors due to the shorter 2nd GC column (comparable to those used for the ultra-fast GC measurements) which elutes samples within just a few seconds. Recently, JEOL has developed a new generation GC-HRTOFMS system called the “AccuTOF GCv 4G”. The AccuTOF GCv 4G has high sensitivity, high resolution, high mass accuracy and high speed data acquisition, all simultaneously. Also JEOL has developed a unique EI/FI combination ion source for this system which provides the capabilities of GC/EI and GC/FI measurements without having to break vacuum in order to switch between each ionization mode. Additionally, this combination is particularly powerful in that it provides library searchable fragmentation information by using EI and high mass accuracy molecular ion information by using FI.
• Automated Exact Mass Measurements and Elemental Composition Determinations

  The JEOL AccuTOF™ LC/MS system offers easy exact-mass measurements and elemental composition determinations. A robust design and stable time-of-flight mass analyzer are combined with a detection system that provides high sensitivity and high dynamic range. Unlike other API/TOF mass spectrometer systems, the AccuTOF™ provides excellent linearity and mass accuracy over a wide range of analyte concentrations. To demonstrate the potential of the AccuTOF™ for automated exact mass measurements, a variety of small-molecule drug samples were measured by using a macro that allows the user to submit samples for unattended elemental composition determinations. Samples were introduced by using the LC autosampler. The macro applied an automatic drift (“lock mass”) correction to the reserpine reference standard and printed out elemental compositions for user-specified elemental limits. The results show high accuracy and stability regardless of sample concentration.