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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‚ÄČng/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

Representative chromatograms of lumefantrine (left) and artesunate (right) in human plasma. (A) Blank plasma, (B) LLOQ, and (C) Real subject sample.
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fig3: Representative chromatograms of lumefantrine (left) and artesunate (right) in human plasma. (A) Blank plasma, (B) LLOQ, and (C) Real subject sample.

Mentions: Representative chromatograms obtained from blank plasma, plasma spiked with lower limit of quantification, and real subject sample for lumefantrine and artesunate are shown in Figure 3. The mean % interference observed at the retention time of analytes between eight different lots of human plasma including haemolysed and lipemic plasma containing heparin as an anticoagulant was calculated and the value was found to be 0.00% and 0.00% for lumefantrine and artesunate, respectively, which was within acceptance criteria. Six replicates of extracted samples at the LLOQ level in one of the plasma sample having least interference at the retention time of lumefantrine were prepared and analyzed. The % CV of the area ratios of these six replicates of samples was 3.38% for lumefantrine confirming that interference does not affect the quantification at the LLOQ level. Utilization of selected product ions for each compound enhanced mass spectrometric selectivity. The product ions of m/z 512 and 261 were concluded to be specific for lumefantrine and artesunate.


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)

Representative chromatograms of lumefantrine (left) and artesunate (right) in human plasma. (A) Blank plasma, (B) LLOQ, and (C) Real subject sample.
© Copyright Policy - open-access
Related In: Results  -  Collection

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

fig3: Representative chromatograms of lumefantrine (left) and artesunate (right) in human plasma. (A) Blank plasma, (B) LLOQ, and (C) Real subject sample.
Mentions: Representative chromatograms obtained from blank plasma, plasma spiked with lower limit of quantification, and real subject sample for lumefantrine and artesunate are shown in Figure 3. The mean % interference observed at the retention time of analytes between eight different lots of human plasma including haemolysed and lipemic plasma containing heparin as an anticoagulant was calculated and the value was found to be 0.00% and 0.00% for lumefantrine and artesunate, respectively, which was within acceptance criteria. Six replicates of extracted samples at the LLOQ level in one of the plasma sample having least interference at the retention time of lumefantrine were prepared and analyzed. The % CV of the area ratios of these six replicates of samples was 3.38% for lumefantrine confirming that interference does not affect the quantification at the LLOQ level. Utilization of selected product ions for each compound enhanced mass spectrometric selectivity. The product ions of m/z 512 and 261 were concluded to be specific for lumefantrine and artesunate.

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‚ÄČng/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