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Determination of residual dimethylsulphoxide in drug loaded gelatin using thermal desorber – gas chromatography

Determination of residual dimethylsulphoxide in drug loaded gelatin using thermal desorber – gas chromatography

Authors :
Kris Wolfs
Adissu Alemayehu Asfaw
Erwin Adams
Ann Van Schepdael
Source :
Journal of Pharmaceutical and Biomedical Analysis. 153:193-198
Publication Year :
2018
Publisher :
Elsevier BV, 2018.

Abstract

Traditional headspace - gas chromatography (HS-GC) methods for the determination of residual solvents (RS) start from a homogenous sample solution. Subsequently, it is challenging to determine RS using HS-GC techniques from insoluble solid samples like gelatin which is practically impossible to dissolve or distribute uniformly in water and common organic solvents. In this study, a thermal desorber combined with capillary gas chromatography and flame ionization detection/mass spectrometry (TD-GC-FID/MS) was used for quantitative determination of residual dimethylsulfoxide (DMSO) in gelatin without sample pretreatment. A sample of gelatin was sandwiched between two quartz filter double layers in a polytetrafluoroethylene insert which was then placed in its entirety into a thermal desorption tube. Factors affecting the performance of TD-GC including desorption time, desorption temperature, desorption flow and type of adsorbent were studied by applying a standard solution of DMSO in methanol on a blank gelatin bed. Validation results of the proposed method showed good linearity with an R2-value higher than 0.999 for a wide concentration range and good sensitivity with a limit of detection and limit of quantification of 0.1 μg and 0.2 μg on tube, respectively. The proposed method shows recovery values close to 100%. In addition, a conventional HS-GC method following enzymatic degradation of gelatin was developed to verify the proposed TD-GC method. Both methods were applied for the determination of residual DMSO in gelatin that was loaded with an experimental drug. Results were comparable, but the enzyme assisted HS-GC method was more time consuming and expensive. ispartof: JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS vol:153 pages:193-198 ispartof: location:England status: published

Details

ISSN :
07317085
Volume :
153
Database :
OpenAIRE
Journal :
Journal of Pharmaceutical and Biomedical Analysis
Accession number :
edsair.doi.dedup.....84da9a31b411a8460a9f6e195dd9ce50
Full Text :
https://doi.org/10.1016/j.jpba.2018.02.047