药用胶塞中二甲基环体硅氧烷残留量及在药品中迁移量的测定

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

目的:针对胶塞中二甲基环体硅氧烷具有潜在毒性,建立气相色谱法测定药用胶塞中六甲基环三硅氧烷(hexamethyl cyclotrisiloxane,D3)、八甲基环四硅氧烷(octamethyl cyclotetrasiloxane,D4)、十甲基环五硅氧烷(decamethyl cyclopentasiloxane,D5)和十二甲基环六硅氧烷(dodecamethyl cyclohexasiloxane,D6)的残留量,考察其在注射用头孢类药品中的迁移情况。方法:色谱柱采用DB-WAX毛细管柱(30 m×0.320 mm×0.25μm);载气为N2,进样体积1μL,柱流量1.5 mL·min^(-1),分流比10∶1;色谱柱温度采用程序升温,初始温度35℃,保持5 min,以10℃·min^(-1)升温至180℃,再以50℃·min^(-1)升温至240℃,保持5 min;进样口温度为250℃;检测器为FID,温度250℃。结果:4种二甲基环体硅氧烷质量浓度在1.0~25.0μg·mL-1范围内线性关系良好(r≥0.9997),检测限分别为0.51、0.50、0.52、0.52μg·mL-1,平均回收率分别为93.8%、95.7%、95.6%、95.2%。溴化丁基胶塞中D3、D4、D5最高含量分别为15.74、21.42、11.36μg·g-1,迁移药品中D5最高含量为23.97μg·g-1。结论:该方法灵敏度高,结果准确,重现性好,可用于药用胶塞中二甲基环体硅氧烷测定及迁移研究。

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×0.25μm)was used.The carrier gas was nitrogen and the volume of injection was 1μL.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:Thefour kinds of dimethyl cyclosiloxane had a good linear relationship(r≥0.9997)in the range of 1.0-25.0μg·mL-1.The limit of detection was 0.51,0.50,0.52,and 0.52μg·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 11.36μg·g-1,respectively.The migration of D5 was 23.97μg·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.