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Determination of octreotide and assessment of matrix effects in human plasma using ultra high performance liquid chromatography-tandem mass spectrometry
Faculty
Pharmacy
Year:
2011
Type of Publication:
Article
Pages:
2081-2088
Authors:
Ismaiel, Omnia A, Karnes, H. Thomas, Jenkins, Rand, Zhang, Tianyi
DOI:
10.1016/j.jchromb.2011.05.039
Journal:
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES ELSEVIER SCIENCE BV
Volume:
879
Research Area:
Biochemistry \& Molecular Biology; Chemistry
ISSN
ISI:000293262500010
Keywords :
Oncology, UPLC, Peptide, Ion suppression, Micro elution, Cancer, Phospholipids
Abstract:
A selective UHPLC-MS/MS method for determination of the therapeutic peptide octreotide in human plasma was developed and validated. This assay used a UHPLC C(18) column with 1.7 mu m particle size for efficient separation and an ion-exchange SPE for selective extraction. Octreotide and its labeled internal standard, {[}(13)C(6)Phe(3)] octreotide, were extracted from human plasma using a simple Oasis (R) WCX mu Elution SPE method and analyzed with a total chromatographic run time of 7.5 min. Matrix effects were studied during method development by direct monitoring of representative phospholipids. On-line removal of phospholipids using column switching and pre-column back-flushing was carried out to trap and remove any residual phospholipid matrix interferences. The UHPLC column provided baseline separation between the analyte and matrix peaks. The chromatographic conditions yielded optimal retention and excellent peak shape for both the analyte and internal standard. The assay was linear in the concentration range of 0.025-25.0 ng/ml, inter- and intra-assay precision and accuracy were within 6.1\% and +/-1.93\%, respectively. Recovery was similar to 73\%. Post-extraction addition experiments showed that matrix effects were less than 4\%. This method for octreotide in human plasma has been validated and utilized to support of clinical pharmacokinetic studies. (C) 2011 Elsevier B.V. All rights reserved.
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