ABSTRACT
Objective To establish an HPLC method for determination of the content of radiosensitizer YABQ and its related substances.Methods Diamonsil C18 column (250 mm ×4.6 mm,5 μm) was used.The mobile phase consisted of methanol-0.1%formic acid (22∶78) and isocratic elution at a flow rate of 1.0 ml/min.The detection wavelength was 266 nm,the temperature of the column was 30℃, and the injection volume was 10 μl.Results The linear range of YABQ was 7-84 μg/ml, r=0.9992.The detection limit was 8 ng (S/N≥3), and the quantitation limit was 24 ng (S/N≥10). According to destructive sample processing, the separation coefficient between the peaks was above 1.5, indicating that this chromatographic method could meet the YABQ monitoring requirements.Conclusion Method validation and destructive testing show that both the precision and specificity are fine with this method, which could be used for quality control of YABQ and its related substances.
ABSTRACT
Objective To establish a headspace gas chromatography method for determination of nine residual solvents in grape seed extract. Methods The residual solvents in grape seed extract were separated on DB-WAX column (30 m× 0.45 mm, 0.85 μm) with an FID detector; the injector temperature and the detector temperature was set at 220 ℃ and 250 ℃ , respectively; the chapiter pressure was 27.58 kPa; the containers of headspace injector were in equilibrium for 30 min at 80 ℃ ;the N, N-dimethylformamide was used as the solvent. Results The detected solvents were well separated. Good linear relationship of the benzene and ethanol was obtained within the range of 0.04-0.3,100-750 μg?mL-1 , respectively. Good linear relationships of the hexane, o-xylene, m-xylene, p-xylene, styrene, toluene and 1,2-diethyl benzene solvents were obtained within the range of 0.4-3.0 μg?mL-1 (r≥0.995 8), respectively. The average recoveries (n = 3) of the nine solvents were 96.35%,97.08%,97.31%,89.93%,92.35%,90.65%,88.56%,93.84%,86.51% and the RSDs were 4.38%,2.16%,3.49%, 4.19%,4.80%,4. 83%,4. 70%,5. 00%,4. 39%, respectively. Conclusion The established method is simple, rapid and accurate, which can be used for the determination of residual solvents in grape seed extract and can simultaneously provide scientific basic for quality control.