Skip to Content
Merck
  • Water determination in active pharmaceutical ingredients using ionic liquid headspace gas chromatography and two different detection protocols.

Water determination in active pharmaceutical ingredients using ionic liquid headspace gas chromatography and two different detection protocols.

Journal of pharmaceutical and biomedical analysis (2014-02-25)
Lillian A Frink, Choyce A Weatherly, Daniel W Armstrong
ABSTRACT

A rapid, accurate, precise and versatile analytical method was developed for the detection and quantification of water in solid active pharmaceutical ingredients (APIs). The headspace gas chromatography (HSGC) method utilized an ionic liquid (IL) based open tubular capillary GC column to increase sensitivity and ruggedness of this method. ILs are also utilized as the headspace solvent because of their low vapor pressure, unique physiochemical properties and high thermal stability. This method is not affected by side reactions and solubility problems which are common with Karl Fischer Titration (KFT) methods. Nor is it as limited as weight loss on drying approaches. The ability to use either/both modern thermal conductivity or barrier ion discharge GC detection provides flexibility, different dynamic ranges and sensitivity. The developed method also was shown to be broadly applicable.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
(±)-Ketamine hydrochloride, solid
Sigma-Aldrich
DL-Homocysteine thiolactone hydrochloride, ≥99.0% (AT)
Supelco
Ascorbic Acid, Pharmaceutical Secondary Standard; Certified Reference Material
USP
Ascorbic acid, United States Pharmacopeia (USP) Reference Standard
Ascorbic acid, European Pharmacopoeia (EP) Reference Standard
USP
Verapamil hydrochloride, United States Pharmacopeia (USP) Reference Standard
Verapamil hydrochloride, European Pharmacopoeia (EP) Reference Standard
Supelco
Sodium Tartrate Dihydrate, Pharmaceutical Secondary Standard; Certified Reference Material
Rifampicin, European Pharmacopoeia (EP) Reference Standard
Supelco
Ibuprofen, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Ibuprofen
Sigma-Aldrich
L-Ascorbic acid, 99%
Sigma-Aldrich
L-Ascorbic acid, FCC, FG
Supelco
Warfarin, PESTANAL®, analytical standard
Supelco
L-Ascorbic acid, analytical standard
Supelco
(±)-Verapamil hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
L-Ascorbic acid, puriss. p.a., ≥99.0% (RT)
Sigma-Aldrich
L-Ascorbic acid, tested according to Ph. Eur.
Sigma-Aldrich
L-Ascorbic acid, puriss. p.a., ACS reagent, reag. ISO, Ph. Eur., 99.7-100.5% (oxidimetric)
Sigma-Aldrich
L-Ascorbic acid, ACS reagent, ≥99%
Sigma-Aldrich
Rifampicin, ≥95% (HPLC), powder or crystals
Sigma-Aldrich
Rifampicin, suitable for plant cell culture, BioReagent, ≥95% (HPLC), powder or crystals
Sigma-Aldrich
Ibuprofen, ≥98% (GC)
Sigma-Aldrich
Ibuprofen, meets USP testing specifications
Sigma-Aldrich
L-Ascorbic acid, reagent grade, crystalline
Sigma-Aldrich
L-Ascorbic acid, BioXtra, ≥99.0%, crystalline
Sigma-Aldrich
L-Ascorbic acid, suitable for cell culture, suitable for plant cell culture, ≥98%
Sigma-Aldrich
L-Ascorbic acid, reagent grade
Sigma-Aldrich
L-Ascorbic acid, powder, suitable for cell culture, γ-irradiated
Sigma-Aldrich
(±)-Verapamil hydrochloride, ≥99% (titration), powder