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Electrospray sample preparation for improved quantitation in matrix-assisted laser desorption/ionization time-of-flight mass spectrometry.
Rapid Commun Mass Spectrom. 1997; 11(16):1785-93.RC

Abstract

The goal of this work is the development of a rapid and objective matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) method for the quantitation of peptides and proteins in human plasma suitable for use in the Good Laboratory Practices (GLP) environment, where the analytical method, validation and pharmacokinetic parameters derived from concentration data will be scrutinized by global regulatory agencies. Electrospray deposition has traditionally been used to prepare thin, uniform samples for a number of techniques, including Cf-252 plasma desorption and secondary ion mass spectrometry. Here the electrospray process of sample application is used to reduce the segregation of analyte from matrix during the sample drying step. The small droplets formed during the electrospray process are found to significantly improve the homogeneity of the sample surface prepared. Experiments comparing the traditional air dried and electrosprayed methods of sample preparation show that the increase in sample homogeneity from electrosprayed samples decreases both the within-sample spot and between-sample spot variability, resulting in a decrease in percent coefficient of variation (%CV) for the recorded MALDI mass spectra. The increase in sample homogeneity permits a more objective use of MALDI-TOFMS as a quantitative analytical method and has led to the development of an assay for the determination of desamino-[8-D-arginine] vasopressin (DDAVP) using arginine vasopressin (AVP) as internal standard in human plasma. The range of quantitation observed (2.0-10 micrograms/mL) is of limited value for bioanalytical application; however, the analysis of neat standards shows lower quantitation limits are easily achieved.

Authors+Show Affiliations

Hensel RR
Rhone-Poulenc Rorer Pharmaceutical, Inc., Collegeville, PA 19426, USA.
King RC
No affiliation info available
Owens KG
No affiliation info available

MeSH

Arginine VasopressinCalibrationDeamino Arginine VasopressinHumansIon ExchangeMicroscopy, Electron, ScanningMicroscopy, FluorescencePlasmaSpectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization

Pub Type(s)

Journal Article

Language

eng

PubMed ID

9375412

Citation

Hensel, R R., et al. "Electrospray Sample Preparation for Improved Quantitation in Matrix-assisted Laser Desorption/ionization Time-of-flight Mass Spectrometry." Rapid Communications in Mass Spectrometry : RCM, vol. 11, no. 16, 1997, pp. 1785-93.
Hensel RR, King RC, Owens KG. Electrospray sample preparation for improved quantitation in matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. Rapid Commun Mass Spectrom. 1997;11(16):1785-93.
Hensel, R. R., King, R. C., & Owens, K. G. (1997). Electrospray sample preparation for improved quantitation in matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. Rapid Communications in Mass Spectrometry : RCM, 11(16), 1785-93.
Hensel RR, King RC, Owens KG. Electrospray Sample Preparation for Improved Quantitation in Matrix-assisted Laser Desorption/ionization Time-of-flight Mass Spectrometry. Rapid Commun Mass Spectrom. 1997;11(16):1785-93. PubMed PMID: 9375412.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Electrospray sample preparation for improved quantitation in matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. AU - Hensel,R R, AU - King,R C, AU - Owens,K G, PY - 1997/1/1/pubmed PY - 1998/1/10/medline PY - 1997/1/1/entrez SP - 1785 EP - 93 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun Mass Spectrom VL - 11 IS - 16 N2 - The goal of this work is the development of a rapid and objective matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) method for the quantitation of peptides and proteins in human plasma suitable for use in the Good Laboratory Practices (GLP) environment, where the analytical method, validation and pharmacokinetic parameters derived from concentration data will be scrutinized by global regulatory agencies. Electrospray deposition has traditionally been used to prepare thin, uniform samples for a number of techniques, including Cf-252 plasma desorption and secondary ion mass spectrometry. Here the electrospray process of sample application is used to reduce the segregation of analyte from matrix during the sample drying step. The small droplets formed during the electrospray process are found to significantly improve the homogeneity of the sample surface prepared. Experiments comparing the traditional air dried and electrosprayed methods of sample preparation show that the increase in sample homogeneity from electrosprayed samples decreases both the within-sample spot and between-sample spot variability, resulting in a decrease in percent coefficient of variation (%CV) for the recorded MALDI mass spectra. The increase in sample homogeneity permits a more objective use of MALDI-TOFMS as a quantitative analytical method and has led to the development of an assay for the determination of desamino-[8-D-arginine] vasopressin (DDAVP) using arginine vasopressin (AVP) as internal standard in human plasma. The range of quantitation observed (2.0-10 micrograms/mL) is of limited value for bioanalytical application; however, the analysis of neat standards shows lower quantitation limits are easily achieved. SN - 0951-4198 UR - https://www.unboundmedicine.com/medline/citation/9375412/Electrospray_sample_preparation_for_improved_quantitation_in_matrix_assisted_laser_desorption/ionization_time_of_flight_mass_spectrometry_ L2 - https://doi.org/10.1002/(SICI)1097-0231(19971030)11:16<1785::AID-RCM78>3.0.CO;2-Q DB - PRIME DP - Unbound Medicine ER -
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