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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
- 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
- Subjects :
- PHARMACEUTICALS
SAMPLES
Clinical Biochemistry
Pharmaceutical Science
02 engineering and technology
Standard solution
01 natural sciences
Gelatin
Analytical Chemistry
law.invention
Limit of Detection
law
Desorption
Drug Discovery
Pharmacology & Pharmacy
Polytetrafluoroethylene
Spectroscopy
Flame Ionization
Thermal desorber - gas chromatography
RANGE
Chemistry
AIR
Temperature
021001 nanoscience & nanotechnology
Pharmaceutical Preparations
Physical Sciences
0210 nano-technology
Life Sciences & Biomedicine
CAPSULES
DESORPTION
food.ingredient
Thermal desorption
VOLATILE ORGANIC-COMPOUNDS
Mass spectrometry
Sensitivity and Specificity
Gas Chromatography-Mass Spectrometry
food
Humans
Flame ionization detector
Dimethyl Sulfoxide
SOLVENTS
Detection limit
Science & Technology
Chromatography
Chemistry, Analytical
010401 analytical chemistry
Residual DMSO
0104 chemical sciences
Solvents
Gas chromatography
Subjects
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