Safety Monitoring

Determinnation of residual dimethyl cyclosiloxane and its migration of medicinal rubber stopper*

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  • Chongqing Institute for Food and Drug Control, Chongqing 401121, China

Received date: 2022-08-17

  Online published: 2024-06-25

Abstract

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.

Cite this article

WU Hong-yang . Determinnation of residual dimethyl cyclosiloxane and its migration of medicinal rubber stopper*[J]. Chinese Journal of Pharmaceutical Analysis, 2022 , 42(11) : 1972 -1979 . DOI: 10.16155/j.0254-1793.2022.11.14

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