眼用硅油重均相对分子质量及其寡聚硅氧烷含量分析

Analysis of weight-average relative molecular mass and oligomeric siloxane content for ophthalmic silicone oil

采用凝胶渗透色谱与多角度激光光散射联用仪测定眼用硅油的重均相对分子质量,用气相色谱–质谱联用仪对其低聚物(寡聚硅氧烷类物质)进行定性定量分析。以八甲基环四硅氧烷(D4)、十甲基环五硅氧烷(D5)作为寡聚硅氧烷代表进行检测研究。硅油的重均相对分子质量(Mw)为31KD,相对分子质量分布系数Mw/Mn为2.9。D4,D5的质量浓度分别在1~50μg/mL,2~60μg/mL范围内与其色谱峰面积呈良好的线性,线性相关系数(r^2)分别为0.999,0.998,检出限分别为0.10,0.23μg/mL,D4,D5的加标回收率分别为90.7%~96.7%,87.3%~94.1%。重均相对分子质量及D4,D5测定结果的相对标准偏差均小于5%(n=6)。该方法干扰少,准确度高,可用于眼用硅油质量控制。

The weight average relative molecular mass of ophthalmic silicone oil were identified by gel permaetion chromatography combined with multi angle laser light scattering hyphenator. The oligomer(oligomeric siloxanes) in ophthalmic silicone oil was detected by gas chromatography–mass spectrometry. Octamethyl cyclotetrasiloxane (D4) and decamethyl cyclopentasiloxane (D5) as representatives of oligomeric siloxane were determined and studied. The average relative molecular mass (Mw) of silicone oil was 31 KD and the relative molecular mass distribution coefficient (Mw/Mn) was 2.9. The mass concentration of D4,D5 was linear with its chromatographic peak area in the range of 1–50,2–60 μg/mL,respectively,the linear correlation coefficients(r^2) were 0.999,0.998,and the detection limits were 0.10,0.23 μg/mL,respectively. The recoveries of D4,D5 were 90.7%–96.7%,87.3%–94.1%,respectively. The relative standard deviation of detectiong results was less than 5%(n=6). This method has less interference and high accuracy,which can be used for quality control of ophthalmic silicone oil.