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Quantitative analysis of ezetimibe in human plasma by gas chromatography-mass spectrometry.
J Sep Sci. 2009 Jun; 32(11):1868-74.JS

Abstract

A new, specific and sensitive GC-MS method with electron impact ionization technique was developed for quantitative analysis of ezetimibe (EZE) in human plasma. Prior to GC analysis, EZE was derivatized with N-methyl-N-trimethylsilyl-trifluoroacetamide (MSTFA), which is a trimethyl silylating reagent. The derivatization reaction was optimized and parameters such as catalyst, derivatization time, temperature, solvent and the volume of silylating reagent were investigated. Trimethylsilyl ether derivative of EZE was determined in selected ion monitoring (SIM, mass-to-charge ratio (m/z): 326) mode. The method was validated with respect to LOD and LOQ, precision, accuracy, linearity, specificity, stability, and recovery. The LOQ and LOD were found as 15 and 10 ng/mL, respectively. The linearity of the method ranged from 15 to 250 ng/mL. The correlation coefficient of the calibration curve was 0.9977 +/- 0.0004 (+/- S.E.M.). The intra- and inter-day precisions (RSD) were less than 6% and accuracies (bias) for intra- and inter-day accuracy were found between -4.04 and 9.71% at four different concentration levels (15, 40, 100, 250 ng/mL). The proposed method was successfully applied to real human plasma samples for determination of total EZE.

Authors+Show Affiliations

Department of Basic Pharmaceutical Sciences, Faculty of Pharmacy, Hacettepe University, Ankara, Turkey. ebruu@hacettepe.edu.trNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

19479777

Citation

Uçaktürk, Ebru, et al. "Quantitative Analysis of Ezetimibe in Human Plasma By Gas Chromatography-mass Spectrometry." Journal of Separation Science, vol. 32, no. 11, 2009, pp. 1868-74.
Uçaktürk E, Ozaltin N, Kaya B. Quantitative analysis of ezetimibe in human plasma by gas chromatography-mass spectrometry. J Sep Sci. 2009;32(11):1868-74.
Uçaktürk, E., Ozaltin, N., & Kaya, B. (2009). Quantitative analysis of ezetimibe in human plasma by gas chromatography-mass spectrometry. Journal of Separation Science, 32(11), 1868-74. https://doi.org/10.1002/jssc.200900078
Uçaktürk E, Ozaltin N, Kaya B. Quantitative Analysis of Ezetimibe in Human Plasma By Gas Chromatography-mass Spectrometry. J Sep Sci. 2009;32(11):1868-74. PubMed PMID: 19479777.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Quantitative analysis of ezetimibe in human plasma by gas chromatography-mass spectrometry. AU - Uçaktürk,Ebru, AU - Ozaltin,Nuran, AU - Kaya,Baris, PY - 2009/5/30/entrez PY - 2009/5/30/pubmed PY - 2009/9/2/medline SP - 1868 EP - 74 JF - Journal of separation science JO - J Sep Sci VL - 32 IS - 11 N2 - A new, specific and sensitive GC-MS method with electron impact ionization technique was developed for quantitative analysis of ezetimibe (EZE) in human plasma. Prior to GC analysis, EZE was derivatized with N-methyl-N-trimethylsilyl-trifluoroacetamide (MSTFA), which is a trimethyl silylating reagent. The derivatization reaction was optimized and parameters such as catalyst, derivatization time, temperature, solvent and the volume of silylating reagent were investigated. Trimethylsilyl ether derivative of EZE was determined in selected ion monitoring (SIM, mass-to-charge ratio (m/z): 326) mode. The method was validated with respect to LOD and LOQ, precision, accuracy, linearity, specificity, stability, and recovery. The LOQ and LOD were found as 15 and 10 ng/mL, respectively. The linearity of the method ranged from 15 to 250 ng/mL. The correlation coefficient of the calibration curve was 0.9977 +/- 0.0004 (+/- S.E.M.). The intra- and inter-day precisions (RSD) were less than 6% and accuracies (bias) for intra- and inter-day accuracy were found between -4.04 and 9.71% at four different concentration levels (15, 40, 100, 250 ng/mL). The proposed method was successfully applied to real human plasma samples for determination of total EZE. SN - 1615-9314 UR - https://www.unboundmedicine.com/medline/citation/19479777/Quantitative_analysis_of_ezetimibe_in_human_plasma_by_gas_chromatography_mass_spectrometry_ DB - PRIME DP - Unbound Medicine ER -