Document Detail

Measurement of ethyl methanesulfonate in human plasma and breast milk samples using high-performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry.
MedLine Citation:
PMID:  20102787     Owner:  NLM     Status:  MEDLINE    
Ethyl methanesulfonate (EMS) is a mesylate ester, which is known to be a potent mutagen, teratogen, and possibly carcinogen. Mesylate esters have been found in pharmaceuticals as contaminants formed during the manufacturing process and may potentially pose an exposure hazard to humans. We have developed and validated a method for detection of trace amounts (ng/ml levels) of EMS in human plasma and breast milk. The samples were extracted by matrix solid-phase dispersion with ethyl acetate using Hydromatrix and the ASE 200 Accelerated Solvent Extractor. The extracts were separated by high-performance liquid chromatography (HPLC) using a HILIC column. The detection was performed with a triple quadrupole mass spectrometer (TSQ Quantum Ultra, Thermo Electron Corporation) using atmospheric pressure chemical ionization in negative-ion mode and multiple reaction monitoring. The use of a surrogate internal standard in combination with HPLC-MS/MS provided a high degree of accuracy and precision. The extraction efficiency was greater than 70%. Repeated analyses of plasma and breast milk samples spiked with high (100 ng/ml), medium (50 ng/ml) and low (5 ng/ml) concentrations of the analytes gave relative standard deviations of less than 12%. The limits of detection were in the range of 0.5-0.9 ng/ml for both matrices.
M Angela Montesano; Ralph D Whitehead; Nayana K Jayatilaka; Peter Kuklenyik; Mark D Davis; Larry L Needham; Dana Boyd Barr
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Publication Detail:
Type:  Journal Article     Date:  2010-01-11
Journal Detail:
Title:  Journal of pharmaceutical and biomedical analysis     Volume:  52     ISSN:  1873-264X     ISO Abbreviation:  J Pharm Biomed Anal     Publication Date:  2010 Jun 
Date Detail:
Created Date:  2010-02-17     Completed Date:  2010-05-24     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  8309336     Medline TA:  J Pharm Biomed Anal     Country:  England    
Other Details:
Languages:  eng     Pagination:  260-4     Citation Subset:  IM    
Copyright Information:
Published by Elsevier B.V.
Centers for Disease Control and Prevention, National Center for Environmental Health, Division of Laboratory Sciences, Atlanta, GA 30341, USA.
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MeSH Terms
Atmospheric Pressure
Chromatography, High Pressure Liquid / methods*
Ethyl Methanesulfonate / blood*,  chemistry
Limit of Detection
Milk, Human / chemistry*
Molecular Structure
Molecular Weight
Mutagens / analysis*
Quality Control
Reference Standards
Reproducibility of Results
Sensitivity and Specificity
Tandem Mass Spectrometry / methods*
Reg. No./Substance:
0/Mutagens; 62-50-0/Ethyl Methanesulfonate

From MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine

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