Objective: To establish a gas chromatography method that could determine the residual hexamethyl cyclotrisiloxane(D3)、octamethyl cyclotetrasiloxane(D4)、decamethyl cyclopentasiloxane(D5)、dodecamethyl cyclohexasiloxane(D6) with potentially toxic in the medical rubber stopper and their migration in cephalosporins for injection. Methods: The DB-WAX capillary column(30 m×0.320 mm×0.25 μm)was used. The carrier gas was nitrogen and the volume of injection was 1 μL. The column flow rate was 1.5 mL·min-1 and the split ratio was 10∶1. Column temperature was first kept at 35 ℃ for 5 minutes, then raised to 180 ℃ with the rate of 10 ℃·min-1, then raised to 240 ℃ with the rate of 50 ℃·min-1 and maintained for 5 minutes. The temperature of the gasification chamber was 250 ℃. The detector was FID and the temperature was 250 ℃. Results: The four kinds of dimethyl cyclosiloxane had a good linear relationship(r≥0.999 7) in the range of 1.0-25.0 μg·mL-1. The limit of detection was 0.51, 0.50, 0.52, and 0.52 μg·mL-1, respectively. The average recovery was 93.8%, 95.7%, 95.6%, and 95.2%, respectively. The highest content of D3, D4 and D5 in bromobutyl rubber stopper was 15.74, 21.42, and 11.36 μg·g-1, respectively. The migration of D5 was 23.97 μg·g-1. Conclusion: The method is accurate with high sensitivity and good repeatability, which can be used for the assay of dimethyl cyclosiloxane and their migration in medicinal rubber stopper.
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