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Citation: MA Bo-Kai, Gao Xia, LIU Wei-Li, LIN Yu-Qing. Simultaneous Determination of Six Residual Solvents in Topiroxostat by Headspace Gas Chromatography[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(10): 1528-1532. doi: 10.11895/j.issn.0253-3820.160321 shu

Simultaneous Determination of Six Residual Solvents in Topiroxostat by Headspace Gas Chromatography

MA Bo-Kai ^1,2, ,
Gao Xia ² ,
LIU Wei-Li ² ,
LIN Yu-Qing ¹

1.
Department of Chemistry, Capital Normal University, Beijing 100048, China;
2.
Beijing Key Laboratory of Detection Technology and Quality Evaluation of Organic Materials, Beijing Center for Physical and Chemical Analysis, Beijing 100089, China

Received Date: 22 April 2016
Revised Date: 9 August 2016

Figures(3)

A simple and sensitive headspace gas chromatographic method was developed and validated for simultaneous determination of methanol, ethanol, dichloromethane, ethyl acetate, 1,4-dioxane and pyridine in topiroxostat. Under the conditions of optimization of stationary phase, heating temperature and equilibration time, the separation was achieved on a Rtx-200 column (30 m×0.25 mm×1 μm) filled with polytrifluoropropyl(methyl) siloxane by a flame ionization detector. The developed gas chromatographic method offered symmetric peak shape, and good resolution for all the 6 solvents. The good linearity was obtained for all the analytes with the correlation coefficients (R²) greater than 0.998. The limits of quantification were 0.006% for methanol, 0.005% for ethanol, 0.012% for dichloromethane, 0.0025% for ethyl acetate, 0.0076% for 1,4-dioxane and 0.004% for pyridine, respectively. The recoveries for 6 residual solvents at three spiked levels were in the range of 92.3%-100.3% with relative standard deviations of 0.32%-3.6%. The real sample analyses showed that this method was simple, fast and feasible for the simultaneous determination of 6 residual solvents in topiroxostat.
- Headspace gas chromatography,
- Topiroxostat,
- Residual solvents,
- Simultaneous determination
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