Journal
JOURNAL OF SEPARATION SCIENCE
Volume 32, Issue 11, Pages 1965-1974Publisher
WILEY PERIODICALS, INC
DOI: 10.1002/jssc.200800644
Keywords
beta(2)-Agonists; Electrospray ionization mass spectrometry; Hydrophilic interaction chromatography; Polymer monolith microextraction; Urine
Categories
Funding
- National Science Fund for Distinguished Young Scholars [20625516]
- National Key Technologies RD Program [2006BAF07B03]
- Science Fund for Creative Research Groups [20621502]
- NSFC
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An analytical method based on online combination of polymer monolith microextraction (PMME) technique with hydrophilic interaction LC (HILIC)/MS is presented. The extraction was performed with a poly(methacrylic acid-co-ethylene glycol dimethacrylate) monolithic column while the subsequent separation was carried out on a Luna silica column by HILIC. After 1:1 v/v dilution with 20 mM phosphate solution at pH 7.0 and centrifugation, urine sample was directly used for extraction. After optimization, 85% ACN (containing 0.3% formic acid v/v) was used for rapid online elution, which was also the mobile phase in HILIC to avoid band broadening during separation or carry-over that was usually observed in PMME-RP LC system. Online automation of extraction and separation procedures was realized under the control of a program in this study. The developed method was applied to rapid and sensitive monitoring of three beta(2)-agonist traces in human urine. The LODs (S/N = 3) of the method were found to be 0.05 - 0.09 ng/mL of beta(2)-agonists in urine. The recoveries of three beta(2)-agonists spiked in five different urine samples ranged from 79.8 to 119.8%, with RSDs less than 18.0%.
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