Validation of new instrumentation for isotope dilution mass spectrometric determination of organic serum analytes

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J Res Natl Inst Stand Technol | / 2卷 / 141-145期

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A major activity in the 20 year collaboration between the Analytical Chemistry Division at NIST and the College of American Pathologists (CAP) has been the development of highly accurate and precise `definitive' methods for important clinical analytes in human serum. Definitive methods for organic analytes use isotope dilution/gas chromatography/mass spectrometry and require a mass spectrometer capable of making highly precise measurements of the ratio between the ion intensities of a characteristic ion from the analyte of interest and its stable-isotope-labeled analog. Recently, the mass spectrometer used for 20 years for definitive method development and measurements was replaced with a modern instrument capable of automated operation, with accompanying gains in convenience and sample throughput. Switching to the new instrument required modifications of measurement protocols, acceptance criteria, and ratio calculations with background corrections to go along with automated instrument operation. Results demonstrated that the two instruments gave comparable results for measurements of both urea and cholesterol in samples from various serum-based Standard Reference Materials [SRMs] and College of American Pathologists materials.

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