MilliporeSigma
  • Development and validation of an ultrafiltration-UPLC-MS/MS method for rapid quantification of unbound docetaxel in human plasma.

Development and validation of an ultrafiltration-UPLC-MS/MS method for rapid quantification of unbound docetaxel in human plasma.

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences (2014-07-27)
Ping Du, Xiaohong Han, Ning Li, Hongyu Wang, Sheng Yang, Yuanyuan Song, Yuankai Shi
ABSTRACT

Docetaxel lipid microsphere (DT-LM) is a novel formulation of docetaxel without Tween-80. A sensitive, robust and reproducible ultrafiltration (UF) followed by UPLC-MS/MS method was developed and validated for the quantification of unbound docetaxel in human plasma using paclitaxel as IS. Ultrafiltrate samples were chromatographed on Acquity UPLC BEH C18 column (50 mm × 2.1 mm, 1.7 μm). The mobile phase was a mixture of 10mM ammonium formate in water containing 0.2% formic acid (A) and acetonitrile containing 0.2% formic acid (B). The volume of plasma utilized was only 450 μL. The calibration curve was linear over the range of 0.2-200 ng/mL, with LLOQ of 0.2 ng/mL. The method was shown to be reliable and reproducible with intra- and inter-day precision and accuracy <±15%, and extraction recovery of 98.1-104.8%. Docetaxel was stable during stability studies, e.g., short term, post-preparation and freeze-thaw cycles. The validated method was utilized to support the pharmacological study of DT-LM in patients with advanced cancer.

MATERIALS
Product Number
Brand
Product Description

Supelco
Residual Solvent - Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Formic acid, puriss., meets analytical specifications of DAC, FCC, 98.0-100%
Sigma-Aldrich
Formic acid, reagent grade, ≥95%
Sigma-Aldrich
Formic acid, ACS reagent, ≥96%
Sigma-Aldrich
Formic acid, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥98%
Sigma-Aldrich
Formic acid, ≥95%, FCC, FG
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (w/v) ammonium formate, 5 % (v/v) water, 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
Acetonitrile solution, contains 10.0% acetone, 0.05% formic acid, 40.0% 2-propanol
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (v/v) trifluoroacetic acid
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Supelco
Methanol solution, contains 0.10 % (v/v) formic acid, UHPLC, suitable for mass spectrometry (MS), ≥99.5%
Sigma-Aldrich
tert-Butyl methyl ether, puriss. p.a., ≥99.5% (GC)
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, Absolute - Acetone free
Sigma-Aldrich
Acetonitrile, ReagentPlus®, 99%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
tert-Butyl methyl ether, reagent grade, ≥98%
Sigma-Aldrich
Methanol, Laboratory Reagent, ≥99.6%
Sigma-Aldrich
Ammonium formate, reagent grade, 97%
Sigma-Aldrich
Methanol, ACS spectrophotometric grade, ≥99.9%
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
tert-Butyl Methyl Ether, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%, poly-coated bottles
Supelco
Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
USP
Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Ammonium formate, BioUltra, ≥99.0% (calc. based on dry substance, NT)
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, 99.93%
Sigma-Aldrich
Formic acid solution, BioUltra, 1.0 M in H2O