A highly sensitive fluorimetric method for determination of lenalidomide in its bulk form and capsules via derivatization with fluorescamine

Darwish, Ibrahim A.; Khalil, Nasr Y.; Bakheit, Ahmed H.; Alzoman, Nourh Z

doi:10.1186/1752-153x-6-118

Cited by 12 publications

(8 citation statements)

References 14 publications

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“…Calculations on 6 replicate experimental injections, the LOD and LOQ were 0.8 and 2.3 ng/mL respectively, and the relative standard deviations (RSD) did not exceed 2%. The LOD achieved in this method was lower than that achieved in our previous method involving the same derivatization procedure [32]. This is attributed due to the difference in the detection systems between the conventional fluorimeter (in the previous study) and the fluorescence HPLC detector in the method described herein.…”

Section: Resultsmentioning

confidence: 67%

“…From our previous study of the reaction between LND and FLC [32], we found that the reaction was dependent on FLC concentration, pH of the reaction medium, the nature of the diluting solvent and the duration of the reaction time. The investigations revealed that the best conditions for the reaction were found by maintaining a final concentration of 0.0025% w/v of FLC, a neutral pH using simple water as diluting solvent and leaving the reaction to proceed for five minutes at room temperature.…”

Section: Resultsmentioning

confidence: 99%

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Trace determination of lenalidomide in plasma by non-extractive HPLC procedures with fluorescence detection after pre-column derivatization with fluorescamine

Khalil

Darwish

Wani

et al. 2013

Chemistry Central Journal

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BackgroundLenalidomide (LND) is a new potent drug used for treatment of multiple myeloma. For its pharmacokinetic studies and therapeutic monitoring, a proper analytical method was required.ResultsIn this study, a non extractive and simple pre-column derivatization procedures have been proposed, for the for trace determination of lenalidomide (LND) in human plasma by HPLC with fluorescence detection. Plasma samples were treated with acetonitrile for protein precipitation then treated with copper acetate to form stable complexes with the biogenic amines and mask their interference with the derivatization reaction of LND. Treated plasma samples containing LND was derivatized with fluorescamine (FLC) in aqueous media at ambient temperature. Separation of the derivatized LND was performed on Hypersil BDS C18 column (250 × 4.6 mm, 5 μm particle size) using a mobile phase consisting of phosphate buffer (pH 4):methanol: tetrahydrofuran (70:10:20, v/v) at a flow rate of 1.0 mL/min. The derivatized samples were monitored at an emission wavelength of 495 nm after excitation at a wavelength of 382 nm. Under the optimum chromatographic conditions, a linear relationship with good correlation coefficient (r = 0.9997, n = 9) was found between the peak area and LND concentrations in the range of 2–100 ng/mL. The limits of detection and quantitation were 0.8 and 2.30 ng/mL, respectively. The intra- and inter-assay precisions were satisfactory and the accuracy of the method was proved. The recovery of LND from the spiked human plasma was 99.30 ± 2.88.ConclusionsThe proposed method had high throughput as the analysis involved simple sample pre-treatment procedure and a relatively short run-time (< 15 min). The results demonstrated that the method would have a great value when it is applied in the therapeutic monitoring and pharmacokinetic studies for LND.

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Section: Resultsmentioning

confidence: 67%

Section: Resultsmentioning

confidence: 99%

Trace determination of lenalidomide in plasma by non-extractive HPLC procedures with fluorescence detection after pre-column derivatization with fluorescamine

Khalil

Darwish

Wani

et al. 2013

Chemistry Central Journal

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“…Several chromatographic methods including spectrophotometric [12] and fluorimetric [13] methods were developed for the determination of LENA in pharmaceutical formulations such as bulk materials and capsules. Lopez et.…”

Section: Tdmmentioning

confidence: 99%

A Simple and Rapid LC-MS/MS Method for Therapeutic Drug Monitoring of Lenalidomide

Nesetoglu¹,

Kaplan²,

Aslan³

et al. 2020

Pak J Anal Environ Chem

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Immunomodulatory drugs lenalidomide (LENA) and pomalidomide (POMA) are synthetic compounds derived by modifying the chemical structure of thalidomide to improve its potency and reduce its side effects. LENA is used as a treatment for myeloma and blood disorders called myelodysplastic syndromes. The maximum clinical dose of LENA for some haematological cancers is generally ≤25 mg. Therapeutic drug monitoring (TDM) is important for the individualization of drug dosage. A highly sensitive and high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) assay was developed and validated for the quantification of LENA in human plasma. LENA was extracted from human plasma by liquidliquid extraction by ethyl acetate and analysed using a reversed phase isocratic elution on a Poroshell 120 EC-C18, (4.6 -50 mm, 2.7µm) column. A. 0.1% formic acid: methanol (10:90% v/v), was used as mobile phase and detection was performed by triple quadrupole mass spectrometry LC-MS/MS using jet stream electrospray ionization in negative mode. POMA was used as the internal standard (IS). Analyte and IS were detected by tandem mass spectrometry using multiple reaction monitoring (MRM) of precursor-product ion transitions with 0.100 s dwell time, at m/z 258.0 > 213.0 for LENA and m/z 272.0 > 161.0 for POMA. The calibration curves were consistently accurate and precise over the concentration range of 20 to 1000 ng/mL in plasma for LENA. This novel LC-MS/MS method competes with all the regulatory requirements and shows satisfactory accuracy and precision. It is sufficiently sensitive for the performance of pharmacokinetic, bioequivalence and TDM studies in humans.

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“…In the past years, fluorescence detection has been proposed as an alternative to mass detectors, but LND is not a fluorescent compound so precolumn derivatization with fluorescamine is necessary, which increases time of procedure and variability. 6,7 On the other hand, none of the published methods has a linearity range that allows therapeutic drug monitoring of LND for pharmacokinetic studies. Accordingly, the development of a new alternative analytical method for the determination of LND in plasma with adequate sensitivity and selectivity, low cost, and wider linearity range is needed.…”

Section: Introductionmentioning

confidence: 99%

A Wide Linearity Range Method for the Determination of Lenalidomide in Plasma by High-Performance Liquid Chromatography: Application to Pharmacokinetic Studies

et al. 2016

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A wide linearity range analytical method for the determination of lenalidomide in patients with multiple myeloma for pharmacokinetic studies is required. Plasma samples were ultrasonicated for protein precipitation. A solid-phase extraction was performed. The eluted samples were evaporated to dryness under vacuum, and the solid obtained was diluted and injected into the high-performance liquid chromatography (HPLC) system. Separation of lenalidomide was performed on an Xterra RP C18 (250 mm length × 4.6 mm i.d., 5 µm) using a mobile phase consisting of phosphate buffer/acetonitrile (85:15, v/v, pH 3.2) at a flow rate of 0.5 mL · min The samples were monitored at a wavelength of 311 nm. A linear relationship with good correlation coefficient (r = 0.997, n = 9) was found between the peak area and lenalidomide concentrations in the range of 100 to 950 ng · mL The limits of detection and quantitation were 28 and 100 ng · mL, respectively. The intra- and interassay precisions were satisfactory, and the accuracy of the method was proved. In conclusion, the proposed method is suitable for the accurate quantification of lenalidomide in human plasma with a wide linear range, from 100 to 950 ng · mL This is a valuable method for pharmacokinetic studies of lenalidomide in human subjects.

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A highly sensitive fluorimetric method for determination of lenalidomide in its bulk form and capsules via derivatization with fluorescamine

Cited by 12 publications

References 14 publications

Trace determination of lenalidomide in plasma by non-extractive HPLC procedures with fluorescence detection after pre-column derivatization with fluorescamine

Trace determination of lenalidomide in plasma by non-extractive HPLC procedures with fluorescence detection after pre-column derivatization with fluorescamine

A Simple and Rapid LC-MS/MS Method for Therapeutic Drug Monitoring of Lenalidomide

A Wide Linearity Range Method for the Determination of Lenalidomide in Plasma by High-Performance Liquid Chromatography: Application to Pharmacokinetic Studies

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