眼科手术用硅油中五种小分子物质残留量的测试

GC Simultaneous Determination of Five Kinds of Small Molecular Levels in Silicone Oil

目的：建立一种利用气相色谱法同时测定硅油中5种小分子物质含量的方法。方法：以正己烷为溶剂,采用GC法,色谱柱为Rtx-5MS毛细管色谱柱（30 m×0.25 mm×0.25μm）;柱温采用程序升温（60℃保持3 min,10℃·min-1速率升温至160℃,保持1 min,再以40℃·min-1的速率升温至280℃,保持2 min）;进样口温度：280℃;检测器：FID;检测器温度：280℃。结果：六甲基环三硅氧烷、八甲基三硅氧烷、八甲基环四硅氧烷、十甲基四硅氧烷、十甲基环五硅氧烷分别在1.42～22.80、1.60～25.62、1.78～28.56、1.56～24.90、1.77～28.32μg·m L-1质量浓度范围内与峰面积呈良好线性关系,回收率分别为105.8%、102.6%、103.4%、98.21%、101.0%。结论：该方法准确、可靠、灵敏度高,为硅油中5种小分子物质的测定提供了一种准确实用的分析方法。

Objective： To establish a gas chromatographic method for simultaneous determination of five kinds of small molecular levels in silicone oil. Methods： Using hexane as solvent, the determination was performed on a Rtx-SMS capillary column （30 m×0.25 mm×0.25 ~tm）. The column temperature was maintained at 60 ℃ for 3 min, and programmed to 160 ℃ at the rate of 10 ℃· min 1 for 1 min. After that the temperature was elevated to 280 ℃ at the rate of 40 9℃· min 1 for 2 rain. The FID was used as detector. The temperature of the injection and the detector was both set at 280 ℃ . Results： The concentrations of hexamethylcyclotrisiloxane, octamethyltrisiloxane, octamethylcyclotetrasiloxane, decamethyltetrasiloxane, and decamethylcyclopentasiloxane were ranged in 1.42-22.80, 1.60-25.62, 1.78-28.56, 1.56-24.90, and 1.77-28.32 μg · mL-1 with a good linear relationship between peak areas, respectively. The average recoveries were 105.8%, 102.6%, 103.4%, 98.21%, and 101.0%, respectively. Conclusion： The established method is accurate, reliable, and sensitive, which provides an accurate and practical method for simultaneous determination of five kinds of small molecular levels in silicone oil.