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Quantification of Lumefantrine in Human Plasma Using LC-MS/MS and Its Application to a Bioequivalence Study.

Pingale SG, Mangaonkar KV - J Pharm (Cairo) (2012)

Bottom Line: Artesunate was used as an internal standard for lumefantrine.The overall recovery for lumefantrine and artesunate was 93.16% and 91.05%, respectively.This validated method was used successfully for analysis of plasma samples from a bioequivalence study.

View Article: PubMed Central - PubMed

Affiliation: Analytical Chemistry Research Laboratory, Mithibai College of Arts, Chauhan Institute of Science & Amrutben Jivanlal College of Commerce & Economics, Vile Parle (W), Mumbai 400056, India.

ABSTRACT
An analytical method based on protein precipitation has been developed and validated for analysis of lumefantrine in human plasma. Artesunate was used as an internal standard for lumefantrine. Inertsil ODS column provided chromatographic separation of analytes followed by detection with mass spectrometry. The method involves simple isocratic chromatographic condition and mass spectrometric detection in the positive ionization mode using an API-3000 system. The total run time was 2.5 minutes. The proposed method has been validated with linear range of 200-20000 ng/mL for lumefantrine. The intrarun and interrun precision values are within 6.66% and 5.56%, respectively, for lumefantrine at the lower limit of quantification level. The overall recovery for lumefantrine and artesunate was 93.16% and 91.05%, respectively. This validated method was used successfully for analysis of plasma samples from a bioequivalence study.

No MeSH data available.


Related in: MedlinePlus

Product ion mass spectrum of lumefantrine.
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fig1: Product ion mass spectrum of lumefantrine.

Mentions: Chromatographic separation was carried out on a Shimadzu LC (Kyoto, Japan) with a Inertsil ODS-2V column (50 × 4.6 mm, 5 μm) purchased from GL Sciences Inc., Japan. A mobile phase consisting of methanol, acetonitrile, and 0.1% formic acid in water solution in the ratio of 56 : 24 : 20 v/v/v was delivered with a splitter at a flow rate of 1 mL/min. The total run time for each sample analysis was 2.5 minutes. Mass spectra were obtained using an API-3000 from Applied Biosystems, Canada, equipped with electrospray ionization source. The mass spectrometer was operated in the multiple reaction monitoring (MRM) mode. Electrospray ionization in the positive ion mode was used for sample introduction and ionization. Source-dependent parameters optimized were as follows: nebulizer gas flow: 8 L/min; auxiliary gas flow: 8 L/min; ion spray voltage (ISV): 5500 V, and temperature (TEM): 400°C. The compound-dependent parameters such as the declustering potential (DP), focusing potential (FP), entrance potential (EP), collision energy (CE), cell exit potential (CXP) were optimized during tuning as 100, 360, 10, 41, 10 and 30, 110, 10, 24, 10 eV for lumefantrine and artesunate, respectively. The collision-activated dissociation (CAD) gas was set at 4 psi, while the curtain gas flow was set at 6 L/min using nitrogen gas. Quadrupole 1 and quadrupole 3 were both maintained at unit resolution and dwell time was set at 200 ms for lumefantrine and artesunate. The mass transitions were selected as m/z 530 → 512 for lumefantrine and m/z 407 → 261 for artesunate. The product ion mass spectra for lumefantrine and artesunate are represented in Figures 1 and 2, respectively.


Quantification of Lumefantrine in Human Plasma Using LC-MS/MS and Its Application to a Bioequivalence Study.

Pingale SG, Mangaonkar KV - J Pharm (Cairo) (2012)

Product ion mass spectrum of lumefantrine.
© Copyright Policy - open-access
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC4595938&req=5

fig1: Product ion mass spectrum of lumefantrine.
Mentions: Chromatographic separation was carried out on a Shimadzu LC (Kyoto, Japan) with a Inertsil ODS-2V column (50 × 4.6 mm, 5 μm) purchased from GL Sciences Inc., Japan. A mobile phase consisting of methanol, acetonitrile, and 0.1% formic acid in water solution in the ratio of 56 : 24 : 20 v/v/v was delivered with a splitter at a flow rate of 1 mL/min. The total run time for each sample analysis was 2.5 minutes. Mass spectra were obtained using an API-3000 from Applied Biosystems, Canada, equipped with electrospray ionization source. The mass spectrometer was operated in the multiple reaction monitoring (MRM) mode. Electrospray ionization in the positive ion mode was used for sample introduction and ionization. Source-dependent parameters optimized were as follows: nebulizer gas flow: 8 L/min; auxiliary gas flow: 8 L/min; ion spray voltage (ISV): 5500 V, and temperature (TEM): 400°C. The compound-dependent parameters such as the declustering potential (DP), focusing potential (FP), entrance potential (EP), collision energy (CE), cell exit potential (CXP) were optimized during tuning as 100, 360, 10, 41, 10 and 30, 110, 10, 24, 10 eV for lumefantrine and artesunate, respectively. The collision-activated dissociation (CAD) gas was set at 4 psi, while the curtain gas flow was set at 6 L/min using nitrogen gas. Quadrupole 1 and quadrupole 3 were both maintained at unit resolution and dwell time was set at 200 ms for lumefantrine and artesunate. The mass transitions were selected as m/z 530 → 512 for lumefantrine and m/z 407 → 261 for artesunate. The product ion mass spectra for lumefantrine and artesunate are represented in Figures 1 and 2, respectively.

Bottom Line: Artesunate was used as an internal standard for lumefantrine.The overall recovery for lumefantrine and artesunate was 93.16% and 91.05%, respectively.This validated method was used successfully for analysis of plasma samples from a bioequivalence study.

View Article: PubMed Central - PubMed

Affiliation: Analytical Chemistry Research Laboratory, Mithibai College of Arts, Chauhan Institute of Science & Amrutben Jivanlal College of Commerce & Economics, Vile Parle (W), Mumbai 400056, India.

ABSTRACT
An analytical method based on protein precipitation has been developed and validated for analysis of lumefantrine in human plasma. Artesunate was used as an internal standard for lumefantrine. Inertsil ODS column provided chromatographic separation of analytes followed by detection with mass spectrometry. The method involves simple isocratic chromatographic condition and mass spectrometric detection in the positive ionization mode using an API-3000 system. The total run time was 2.5 minutes. The proposed method has been validated with linear range of 200-20000 ng/mL for lumefantrine. The intrarun and interrun precision values are within 6.66% and 5.56%, respectively, for lumefantrine at the lower limit of quantification level. The overall recovery for lumefantrine and artesunate was 93.16% and 91.05%, respectively. This validated method was used successfully for analysis of plasma samples from a bioequivalence study.

No MeSH data available.


Related in: MedlinePlus