目的 建立液液萃取法测定注射用雷替曲塞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)、十二甲基环六硅氧烷(D6)含量的气相色谱法.方法 采用Agilent CP-Sil 8 CB for Amines毛细管色谱柱(30 m ×0.25 mm,0.5 μm),氢火焰离子化检测器(FID),进样口温度为260 ℃,检测器温度为260 ℃,载气为氮气,流速1.0 mL·min-1,程序升温,直接进样,进样量为1.0 µL,分流比30∶1.结果 4种环硅氧烷类化合物在40～1000 μg·mL-1范围内呈现良好的线性关系,相关系数r为0.9998～0.9999,D3～D6平均加样回收率(n=9)分别为98.45％、96.18％、98.60％、95.14％,RSD分别为1.99％、1.56％、2.72％、0.98％.结论 本文建立注射用雷替曲塞中甲基环硅氧烷的检测方法,本法简便,准确、专属性强,适用于注射用雷替曲塞中环硅氧烷类的检测.
Abstract
OBJECTIVE To establish a GC method for the determination of hexamethyl-cyclotrisiloxane(D3),octamethylcyclotetrasiloxane(D4),decamethylcyclopentasiloxane(D5),dodecamethylcyclohexasiloxane(D6)in Raltitrexed by a liquid-liquid extraction method.METHODS The chromategraphic separation was carried out on the Agilent CP-Sil 8 CB for Amines capillary column(30 m x0.25 mm,0.5 µm).Programmed temperature was ap-plied.The inlet temperature was 260 ℃ and FID detector temperature was 260 ℃.The flow rate of carried gas(N2)was 1.0 mL·min-1 and the split ratio was 30∶1.The injection volume was 1 μL.RESULTS The four dimethylcy-closiloxane volatiles were well separated and showed good linear relationships at the range of 40-1000 μg·mL-1(r is from 0.9998 to 0.9999).The average sample recovery rates(n=9)were 98.45％,96.18％,98.60％,95.14％,and RSD were 1.99％,1.56％,2.72％,and 0.98％,respectively.D3-D6 were not detected in three commercial batches of raltitrexed for injection.CONCLUSION This paper establishes a method for the determination of meth-ylcyclosiloxane in injection product,the method is simple,specific,accurate and suitable for analyzing the residual dimethycuclosiloxane volatiles in Raltitrexed for injection.
关键词
甲基环硅氧烷/硅胶管/注射用雷替曲塞/气相色谱法
Key words
Dimethylcyclosiloxane/Silicon tube/Raltitrexed for injection/GC
维普
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