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  • HPLC method development, validation, and impurity characterization of a potent antitumor indenoisoquinoline, LMP776 (NSC 725776).

HPLC method development, validation, and impurity characterization of a potent antitumor indenoisoquinoline, LMP776 (NSC 725776).

Journal of pharmaceutical and biomedical analysis (2016-03-13)
Jennie Wang, Mingtao Liu, Chun Yang, Xiaogang Wu, Euphemia Wang, Paul Liu
ABSTRACT

An HPLC method for the assay of a DNA topoisomerase inhibitor, LMP776 (NSC 725776), has been developed and validated. The stress testing of LMP776 was carried out in accordance with International Conference on Harmonization (ICH) guidelines Q1A (R2) under acidic, alkaline, oxidative, thermolytic, and photolytic conditions. The separation of LMP776 from its impurities and degradation products was achieved within 40 min on a Supelco Discovery HS F5 column (150 mm × 4.6 mm i.d., 5 μm) with a gradient mobile phase comprising 38-80% acetonitrile in water, with 0.1% trifluoroacetic acid in both phases. LC/MS was used to obtain mass data for characterization of impurities and degradation products. One major impurity was isolated through chloroform extraction and identified by NMR. The proposed HPLC assay method was validated for specificity, linearity (concentration range 0.25-0.75 mg/mL, r = 0.9999), accuracy (recovery 98.6-100.4%), precision (RSD ≤ 1.4%), and sensitivity (LOD 0.13 μg/mL). The validated method was used in the stability study of the LMP776 drug substance in conformance with the ICH Q1A (R2) guideline.

MATERIALS
Product Number
Brand
Product Description

Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 5 cm × 4.6 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 21.2 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 3 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 3 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 2.1 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 3 μm particle size, L × I.D. 2 cm × 4 mm, pkg of 1 kit
Supelco
Discovery® HS F5 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm, pkg of 1 kit
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 5 cm × 4 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 10 cm × 4 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 2.1 mm, pkg of 1 kit
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 15 cm × 4 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 10 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 5 cm × 4.6 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Discovery® HS F5 Supelguard Cartridge, 3 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 15 cm × 2.1 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 10 cm × 4.6 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 3.3 cm × 2.1 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 15 cm × 3 mm, pkg of 1 ea
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
Discovery® HS F5 HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4 mm
Supelco
Discovery® HS F5 HPLC Column, 3 μm particle size, L × I.D. 15 cm × 2.1 mm