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  • Liquid chromatography-mass spectrometry analysis of diethylcarbamazine in human plasma for clinical pharmacokinetic studies.

Liquid chromatography-mass spectrometry analysis of diethylcarbamazine in human plasma for clinical pharmacokinetic studies.

Journal of pharmaceutical and biomedical analysis (2014-07-01)
Mark S Schmidt, Christopher L King, Edward K Thomsen, Peter M Siba, Nelly Sanuku, Lawrence Fleckenstein
ABSTRACT

A sensitive and selective liquid chromatographic method using mass spectrometric detection was developed for the determination of diethylcarbamazine (DEC) in human plasma. DEC and its stable isotope internal standard d3-DEC were extracted from 0.25mL of human plasma using solid phase extraction. Chromatography was performed using a Phenomenex Synergi 4μ Fusion-RP column (2mm×250mm) with gradient elution. The retention time was approximately 4.8min. The assay was linear from 4 to 2200ng/mL. Analysis of quality control samples at 12, 300, and 1700ng/mL (N=15) had interday coefficients of variation of 8.4%, 5.4%, and 6.2%, respectively (N=15). Interday bias results were -2.2%, 6.0%, and 0.8%, respectively. Recovery of DEC from plasma ranged from 84.2% to 90.1%. The method was successfully applied to clinical samples from patients with lymphatic filariasis from a drug-drug interaction study between DEC and albendazole and/or ivermectin.

MATERIALS
Product Number
Brand
Product Description

Supelco
Methanol, analytical standard
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Diethylcarbamazine citrate, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Methanol, NMR reference standard
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, BioReagent, ≥99.93%
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Methanol, Laboratory Reagent, ≥99.6%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, ACS spectrophotometric grade, ≥99.9%
Sigma-Aldrich
Methanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)
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Methanol, puriss., meets analytical specification of Ph Eur, ≥99.7% (GC)
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Methanol, AR, ≥99.5%
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Methanol, suitable for HPLC, ≥99.9%
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Methanol, anhydrous, ≥99.5%
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Methanol, LR, ≥99%
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Methanol, suitable for HPLC, gradient grade, ≥99.9%
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Methanol, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
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Methanol, HPLC Plus, ≥99.9%
USP
Diethylcarbamazine citrate, United States Pharmacopeia (USP) Reference Standard
Supelco
Residual Solvent - Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Methanol, Absolute - Acetone free
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Methanol, ACS reagent, ≥99.8%
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Methanol solution, (Methanol:Dimethyl sulfoxide 1:1 (v/v))
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Acetonitrile, electronic grade, 99.999% trace metals basis
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Methanol solution, contains 0.50 % (v/v) triethylamine
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Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
USP
Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard
USP
Methyl alcohol, United States Pharmacopeia (USP) Reference Standard