气相色谱法测定药用硅橡胶管、硅橡胶垫片中挥发性甲基环硅氧烷的残留量

Determination of residual dimethylcyclosiloxane volatiles in medical silicone rubber tubes and gaskets by GC

目的:建立同时测定药用硅橡胶管、硅橡胶垫片中六甲基环三硅氧烷(D3)、八甲基环四硅氧烷(D4)、十甲基环五硅氧烷(D5)、十二甲基环六硅烷(D6)、十四甲基环七硅氧烷(D7)、十六甲基环八硅氧烷(D8)、十八甲基环九硅氧烷(D9)含量的气相色谱法。方法:采用HP-INNOWAX毛细管气相色谱柱(30 m×0.32 mm,0.50μm),柱温为程序升温,进样口温度230℃,氢火焰离子化检测器(FID)温度250℃,载气N_(2),流速1.0 mL·min^(-1),分流比20∶1,进样量1μL。结果:在选定的色谱条件下,7种挥发性甲基环硅氧烷分离良好,且峰面积与质量浓度呈良好的线性关系(相关系数r均大于0.9990)。D3~D9的平均回收率分别为97.0%、101.4%、97.7%、97.7%、101.7%、100.7%、102.3%。结论:经方法学验证,本法简便,准确、专属性强,适用于药用硅橡胶管、硅橡胶垫片中挥发性甲基环硅氧烷的检测。

Objective:To establish a GC method for the determination of hexamethylcyclotrisiloxane(D3),octamethylcyclotetrasiloxane(D4),decamethylcyclopentasiloxane(D5),dodecamethylcyclohexasiloxane(D6),tetradecamethylcycloheptasiloxane(D7),hexadecamethylcyclooctasiloxane(D8)and octadecamethylcyclononasiloxane(D9)in medical silicone rubber tubes and gaskets.Methods:The chromatographic separation was carried out on the HP-INNOWAX capillary column(30 m×0.32 mm,0.50μm).Programmed temperature was applied.The inlet temperature was 230℃and FID detector temperature was 250℃.The flow rate of carried gas(N;)was 1.0 mL·min^(-1)and the split ratio was 20∶1.The injection volume was 1μL.Results:Under this specific condition,the seven dimethylcyclosiloxane volatiles were well separated and showed good linear relationships between the peak area and the concentration(r>0.9990).The average recoveries of D3-D9 were 97.0%,101.4%,97.7%,97.7%,101.7%,100.7%and 102.3%,respectively.Conclusion:The method issimple,specific,accurate and suitable for analyzing the residual dimethylcyclosiloxane volatiles in medical silicone rubber tubes and gaskets.