Implementation of the chemical reaction interface mass spectrometry technique on a Hewlett-Packard mass-selective detector

Abstract

A microwave-powered chemical reaction interface has been installed in a Hewlett-Packard gas chromatograph-mass spectrometer (GC-MS) system (5890 IT gas chromatograph-S971 mass-selective detector). The technical details and optimization strategies are discussed. The evaluation of this new setup is presented, showing detection limits of 1 ng of (13)C-, (15)N-, and Cl-containing compounds with signal-to-noise ratios greater than or egual to 3. Selective detection was evaluated with a urine sample from a dog dosed with (15)N3-midazolam that had been previously analyzed by using a differentially pumped research-level quadrupole mass spectrometer. The results show that the detection of (15)N and Cl remains highly selective and the mass-selective detector gives comparable sensitivity to the larger instrument when the latter is operating over a conventional mass range. The capability for chemical reaction interface mass spectrometry can be easily accomplished with an inexpensive GC-MS system.

Chemical Reaction Interface Mass Spectrometry with High Efficiency Nebulization

“…CRIMS Instrumentation. The instrumental setup is shown in Figure and is described in detail elsewhere . Briefly, the solution is nebulized and the solvent is removed by desolvation via a heated spray chamber and membrane desolvator (Vestec-Universal Interface).…”

“…The instrumental setup is shown in Figure 1 and is described in detail elsewhere. 29 Briefly, the solution is nebulized and the solvent is removed by desolvation via a heated spray chamber and membrane desolvator (Vestec-Universal Interface). Analyte particles then pass through a momentum separator into a low-pressure MIP (∼ 6 Torr, 70 W forward power, <2 W reflected power, Opthos, Rockville, MD).…”

Pharmacokinetic and metabolism studies using uniformly stable isotope labeled proteins with HPLC/CRIMS detection

“…Samples eluting from the GC column flow directly into the CRI chamber. For these experiments a Hewlett-Packard 5890 Series II gas chromatograph, connected to an HP 5971 mass selective detector were employed [8]. The mass spectrometer has been modified to reduce mass range while increasing transmission and resolution (unpublished work this laboratory).…”

Detection of sulfur‐containing impurities in pharmaceutical samples by high performance liquid chromatography/chemical reaction interface mass spectrometry

“…The result of this high efficiency chemical process is a predictable set of low molecular weight (MW) compounds that are characteristic of the elements contained in the original molecules 2. For example, when nitrogen trifluoride (NF 3 ) is the reactant gas, any carbon contained in the analyte becomes CF 4 and sulfur produces SF 6 3. Conventional electron impact ionisation (EI) mass spectrometry is used to detect these reaction products (as CF 3 + at m/z 69 or SF 5 + at m/z 127).…”