Determination of bis(tributyltin) oxide by GC–MS with on-line hydride derivatization: application to drug substance analysis

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×0.25 mm i.d. DB-5 HT column with a temperature program from 100 to 160°C at 15°C min −1. A mass ra...

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Bibliographic Details
Published in:Journal of pharmaceutical and biomedical analysis 1999-03, Vol.19 (3), p.327-333
Main Authors: O'Brien, Thomas P, Dowling, Thomas M, Moeder, Charles W, Bicker, Gary R
Format: Article
Language:English
Subjects:
Analysis
Biological and medical sciences
Borohydrides - chemistry
Determination of bis(tributyltin) oxide
Drug Contamination - prevention & control
Evaluation Studies as Topic
Gas Chromatography-Mass Spectrometry - instrumentation
Gas Chromatography-Mass Spectrometry - methods
GC–MS determination of tributyltin
General pharmacology
Maximum Allowable Concentration
Medical sciences
On-line hydride derivatization
Organotin Compounds - analysis
Pesticides, fertilizers and other agrochemicals toxicology
Pharmaceutical Preparations - chemistry
Pharmacology. Drug treatments
Reproducibility of Results
Selective-ion monitoring
Sensitivity and Specificity
Toxicology
Trialkyltin Compounds - analysis
Tributyltin chloride
Tributyltin hydride
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Summary: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×0.25 mm i.d. DB-5 HT column with a temperature program from 100 to 160°C at 15°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.
ISSN:0731-7085
1873-264X
DOI:10.1016/S0731-7085(98)00125-3