Determination of bis(tributyltin) oxide by GC–MS with on-line hydride derivatization: application to drug substance analysis
| Autor: | Charles W. Moeder, Thomas P. O'Brien, Thomas Dowling, G. Bicker |
|---|---|
| Rok vydání: | 1999 |
| Předmět: |
Clinical Biochemistry
Pharmaceutical Science chemistry.chemical_element Tributyltin hydride Borohydrides Sensitivity and Specificity Gas Chromatography-Mass Spectrometry Analytical Chemistry chemistry.chemical_compound Tributyltin oxide Drug Discovery Organotin Compounds Derivatization Spectroscopy Detection limit Chromatography Hydride Reproducibility of Results Pharmaceutical Preparations chemistry Evaluation Studies as Topic Tributyltin Maximum Allowable Concentration Gas chromatography Trialkyltin Compounds Drug Contamination Tin |
| Zdroj: | Journal of Pharmaceutical and Biomedical Analysis. 19:327-333 |
| ISSN: | 0731-7085 |
| Popis: | We report the determination of residual bis(tributyltin) oxide in a drug substance by GC-MS after extraction and on-line conversion to tributyltin hydride. Gas chromatography was performed using a 15 m x 0.25 mm i.d. DB-5 HT column with a temperature program from 100 to 160 degrees C at 15 degrees C min(-1). A mass range of 165-185 amu was monitored with the MS detector. Hydride generation is performed by placing a small amount of solid sodium borohydride in the injection port of a gas chromatograph and injecting samples and standards through this material. Conversion to tributyltin hydride is shown to be quantitative and linear for levels of bis(tributyltin) oxide between 1 and 100 ppm in the drug substance. The use of GC-MS provides sensitive and selective detection of tin containing species and the tin isotope pattern allows for confirmation of the presence of tin in chromatographic peaks. Recovery at 6 ppm was 89% with an injection precision of 6%. The limit of detection for bis(tributyltin) oxide in drug substance is 1 ppm. |
| Databáze: | OpenAIRE |
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