A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids

Noorfatimah Yahaya, Mohd Marsin Sanagi, Noorizan Abd Aziz, Wan Aini Wan Ibrahim, Hadi Nur, Saw Hong Loh, Sazlinda Kamaruzaman

Research output: Contribution to journalArticle

Abstract

A rapid dispersive micro-solid phase extraction (D-μ-SPE) combined with LC/MS/MS method was developed and validated for the determination of ketoconazole and voriconazole in human urine and plasma samples. Synthesized mesoporous silica MCM-41 was used as sorbent in d-μ-SPE of the azole compounds from biological fluids. Important D-μ-SPE parameters, namely type desorption solvent, extraction time, sample pH, salt addition, desorption time, amount of sorbent and sample volume were optimized. Liquid chromatographic separations were carried out on a Zorbax SB-C18 column (2.1 × 100 mm, 3.5 μm), using a mobile phase of acetonitrile–0.05% formic acid in 5 mm ammonium acetate buffer (70:30, v/v). A triple quadrupole mass spectrometer with positive ionization mode was used for the determination of target analytes. Under the optimized conditions, the calibration curves showed good linearity in the range of 0.1–10,000 μg/L with satisfactory limit of detection (≤0.06 μg/L) and limit of quantitation (≤0.3 μg/L). The proposed method also showed acceptable intra- and inter-day precisions for ketoconazole and voriconazole from urine and human plasma with RSD ≤16.5% and good relative recoveries in the range 84.3–114.8%. The MCM-41-D-μ-SPE method proved to be rapid and simple and requires a small volume of organic solvent (200 μL); thus it is advantageous for routine drug analysis.

Original languageEnglish
Article numbere3803
JournalBiomedical Chromatography
Volume31
Issue number2
DOIs
StatePublished - 1 Feb 2017

Fingerprint

Ketoconazole
Voriconazole
Butylene Glycols
Amoxicillin
Sorbents
Desorption
Urine
Conjunctival Diseases
Callosities
Acromioclavicular Joint
Pediococcus
Birth Certificates
Mass spectrometers
Solvent extraction
Muscle Contraction
Organic solvents
Ionization
Azoles
Ammonium Compounds
Silicon Dioxide

Keywords

  • dispersive micro-solid phase extraction
  • ketoconazole
  • LC/MS/MS
  • MCM-41
  • voriconazole

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry
  • Molecular Biology
  • Pharmacology
  • Drug Discovery
  • Clinical Biochemistry

Cite this

A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids. / Yahaya, Noorfatimah; Sanagi, Mohd Marsin; Abd Aziz, Noorizan; Wan Ibrahim, Wan Aini; Nur, Hadi; Loh, Saw Hong; Kamaruzaman, Sazlinda.

In: Biomedical Chromatography, Vol. 31, No. 2, e3803, 01.02.2017.

Research output: Contribution to journalArticle

Yahaya, Noorfatimah; Sanagi, Mohd Marsin; Abd Aziz, Noorizan; Wan Ibrahim, Wan Aini; Nur, Hadi; Loh, Saw Hong; Kamaruzaman, Sazlinda / A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids.

In: Biomedical Chromatography, Vol. 31, No. 2, e3803, 01.02.2017.

Research output: Contribution to journalArticle

@article{0c7a19548ad44a739fb86e6d0ddc7864,
title = "A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids",
abstract = "A rapid dispersive micro-solid phase extraction (D-μ-SPE) combined with LC/MS/MS method was developed and validated for the determination of ketoconazole and voriconazole in human urine and plasma samples. Synthesized mesoporous silica MCM-41 was used as sorbent in d-μ-SPE of the azole compounds from biological fluids. Important D-μ-SPE parameters, namely type desorption solvent, extraction time, sample pH, salt addition, desorption time, amount of sorbent and sample volume were optimized. Liquid chromatographic separations were carried out on a Zorbax SB-C18 column (2.1 × 100 mm, 3.5 μm), using a mobile phase of acetonitrile–0.05% formic acid in 5 mm ammonium acetate buffer (70:30, v/v). A triple quadrupole mass spectrometer with positive ionization mode was used for the determination of target analytes. Under the optimized conditions, the calibration curves showed good linearity in the range of 0.1–10,000 μg/L with satisfactory limit of detection (≤0.06 μg/L) and limit of quantitation (≤0.3 μg/L). The proposed method also showed acceptable intra- and inter-day precisions for ketoconazole and voriconazole from urine and human plasma with RSD ≤16.5% and good relative recoveries in the range 84.3–114.8%. The MCM-41-D-μ-SPE method proved to be rapid and simple and requires a small volume of organic solvent (200 μL); thus it is advantageous for routine drug analysis.",
keywords = "dispersive micro-solid phase extraction, ketoconazole, LC/MS/MS, MCM-41, voriconazole",
author = "Noorfatimah Yahaya and Sanagi, {Mohd Marsin} and {Abd Aziz}, Noorizan and {Wan Ibrahim}, {Wan Aini} and Hadi Nur and Loh, {Saw Hong} and Sazlinda Kamaruzaman",
year = "2017",
month = "2",
doi = "10.1002/bmc.3803",
volume = "31",
journal = "Biomedical Chromatography",
issn = "0269-3879",
publisher = "John Wiley and Sons Ltd",
number = "2",

}

TY - JOUR

T1 - A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids

AU - Yahaya,Noorfatimah

AU - Sanagi,Mohd Marsin

AU - Abd Aziz,Noorizan

AU - Wan Ibrahim,Wan Aini

AU - Nur,Hadi

AU - Loh,Saw Hong

AU - Kamaruzaman,Sazlinda

PY - 2017/2/1

Y1 - 2017/2/1

N2 - A rapid dispersive micro-solid phase extraction (D-μ-SPE) combined with LC/MS/MS method was developed and validated for the determination of ketoconazole and voriconazole in human urine and plasma samples. Synthesized mesoporous silica MCM-41 was used as sorbent in d-μ-SPE of the azole compounds from biological fluids. Important D-μ-SPE parameters, namely type desorption solvent, extraction time, sample pH, salt addition, desorption time, amount of sorbent and sample volume were optimized. Liquid chromatographic separations were carried out on a Zorbax SB-C18 column (2.1 × 100 mm, 3.5 μm), using a mobile phase of acetonitrile–0.05% formic acid in 5 mm ammonium acetate buffer (70:30, v/v). A triple quadrupole mass spectrometer with positive ionization mode was used for the determination of target analytes. Under the optimized conditions, the calibration curves showed good linearity in the range of 0.1–10,000 μg/L with satisfactory limit of detection (≤0.06 μg/L) and limit of quantitation (≤0.3 μg/L). The proposed method also showed acceptable intra- and inter-day precisions for ketoconazole and voriconazole from urine and human plasma with RSD ≤16.5% and good relative recoveries in the range 84.3–114.8%. The MCM-41-D-μ-SPE method proved to be rapid and simple and requires a small volume of organic solvent (200 μL); thus it is advantageous for routine drug analysis.

AB - A rapid dispersive micro-solid phase extraction (D-μ-SPE) combined with LC/MS/MS method was developed and validated for the determination of ketoconazole and voriconazole in human urine and plasma samples. Synthesized mesoporous silica MCM-41 was used as sorbent in d-μ-SPE of the azole compounds from biological fluids. Important D-μ-SPE parameters, namely type desorption solvent, extraction time, sample pH, salt addition, desorption time, amount of sorbent and sample volume were optimized. Liquid chromatographic separations were carried out on a Zorbax SB-C18 column (2.1 × 100 mm, 3.5 μm), using a mobile phase of acetonitrile–0.05% formic acid in 5 mm ammonium acetate buffer (70:30, v/v). A triple quadrupole mass spectrometer with positive ionization mode was used for the determination of target analytes. Under the optimized conditions, the calibration curves showed good linearity in the range of 0.1–10,000 μg/L with satisfactory limit of detection (≤0.06 μg/L) and limit of quantitation (≤0.3 μg/L). The proposed method also showed acceptable intra- and inter-day precisions for ketoconazole and voriconazole from urine and human plasma with RSD ≤16.5% and good relative recoveries in the range 84.3–114.8%. The MCM-41-D-μ-SPE method proved to be rapid and simple and requires a small volume of organic solvent (200 μL); thus it is advantageous for routine drug analysis.

KW - dispersive micro-solid phase extraction

KW - ketoconazole

KW - LC/MS/MS

KW - MCM-41

KW - voriconazole

UR - http://www.scopus.com/inward/record.url?scp=85008481895&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=85008481895&partnerID=8YFLogxK

U2 - 10.1002/bmc.3803

DO - 10.1002/bmc.3803

M3 - Article

VL - 31

JO - Biomedical Chromatography

T2 - Biomedical Chromatography

JF - Biomedical Chromatography

SN - 0269-3879

IS - 2

M1 - e3803

ER -