title: Mixed aqueous solutions as dilution media in the determination of residual solvents by static headspace gas chromatography.
abstract: Static headspace (HS) sampling has been commonly used to test for volatile organic chemicals, usually referred to as residual solvents (RS) in pharmaceuticals. If the sample is not soluble in water, organic solvents are used. However, these seriously reduce the sensitivity in the determination of some RS. Here, mixed aqueous dilution media (a mixture of water and an organic solvent like dimethyl formamide, dimethyl sulfoxide or dimethyl acetamide) were studied as alternative media for static HS-gas chromatographic analysis. Although it has been known that mixed aqueous dilution media can often improve sensitivity for many RS, this study used a systematic approach to investigate phase volumes and the organic content in the HS sampling media. Reference solutions using 18 different class 1, 2 and 3 RS were evaluated. The effect of salt addition was also studied in this work. A significant increase in the peak area was observed for all RS using mixed aqueous dilution media, when compared with organic solvents alone. Matrix effects related to the mixed aqueous dilution media were also investigated and reported. Repeatability and linearity obtained with mixed aqueous dilution media were found to be similar to those observed with pure organic solvents.
authors.affiliation: Laboratorium voor Farmaceutische Analyse, Faculteit Farmaceutische Wetenschappen, Katholieke Universiteit Leuven, Leuven, Belgium.
authors.forename: Ward
authors.initials: W
authors.lastname: D'Autry
authors.forename: Chao
authors.initials: C
authors.lastname: Zheng
authors.forename: Kris
authors.initials: K
authors.lastname: Wolfs
authors.forename: Sitaramaraju
authors.initials: S
authors.lastname: Yarramraju
authors.forename: Jos
authors.initials: J
authors.lastname: Hoogmartens
authors.forename: Ann
authors.initials: A
authors.lastname: Van Schepdael
authors.forename: Erwin
authors.initials: E
authors.lastname: Adams
mesh_terms: D000081:Acetamides / Q000737:chemistry*; D002849:Chromatography, Gas; D004121:Dimethyl Sulfoxide / Q000737:chemistry*; D004126:Dimethylformamide / Q000737:chemistry*; D012996:Solutions; D012997:Solvents / Q000032:analysis; D055549:Volatile Organic Compounds / Q000032:analysis*; D014867:Water / Q000737:chemistry*
chemical_list: D000081:Acetamides; D012996:Solutions; D012997:Solvents; D055549:Volatile Organic Compounds; D014867:Water; D004126:Dimethylformamide; D004121:Dimethyl Sulfoxide