气相色谱内标法测定注射级聚山梨酯80中乙二醇、二甘醇、三甘醇残留量

Determination of Glycol,Diglycol and Trithylene Glycol Residues in Injection-grade Polysorbate 80 by GC Internal Standard Method

目的:建立注射级聚山梨酯80中乙二醇、二甘醇、三甘醇残留溶剂检测方法。方法:采用毛细管气相色谱法,以6%氰丙基苯基-94%二甲基聚硅氧烷(DB-624,60 m×0.32 mm×1.8μm)为固定相,柱温为程序升温:初始温度为60℃,以每分钟10℃的速率升温至110℃,维持5 min,再以每分钟40℃的速率升温至170℃,维持5 min;再以每分钟40℃的速率升温至230℃,维持10 min。进样口温度为230℃,检测器温度为250℃;载气(N)流速为5 mL/min。结果:在确定的色谱条件下分离度良好;3种溶剂检测限均满足验证要求,具有良好的线性关系,相关系数(r)均大于0.9990;重复性试验测定结果的RSD(n=6)为2.1%~3.2%,中间精密度试验各溶剂测定结果的RSD(n=12)为1.9%~2.6%;各溶剂回收率为97.2%~100.0%,在80%~120%范围内,且各溶剂结果RSD(n=9)不超过10%。结论:建立的方法专属性强、灵敏度高、有良好的线性关系、精密度和准确度高,可为注射级聚山梨酯80残留溶剂的质量控制提供参考。

Objective:To establish a method for the determination residual solvent for glycol,diglycol and trithylene glycol in injection grade polysorbate 80.Methods:The GC using 6%cyanopropyl phenyl-94%dimethyl polysiloxane(DB-624,60 m×0.32 mm×1.8μm)as the staionary phase.The initial column temperature was 60℃,increasing to 110℃with the speed of 5℃/min and maintained 5 min,speed of 40℃/min and maintained 10 min.The inlet temperature was 230℃and the detector temperature was 250℃.The carrier gas was set at a flow rate of 5 mL/min.Results:The method had good separation with determination of chromatographic conditions.The detection limits of 3 solvent and the quantitation limits were in conformity with verification requirements.Each solvent of the linear relationship was good,and the correlation coefficients were greater than 0.9990.The RSD(n=6)in repeatability test were 2.1%~3.2%,and that RSD(n=12)of each solvent in intermediate precision test were 1.9%~2.6%.The recoveries of each solvent were 94.4%~100.0%,within 80%~120%,and the RSD(n=9)of each solvent were not more than 10%.Conclusion:The method was specificity and has high sensitive,good linear relationship,high precise and accurate,which can give a reference for quality control of residual solvent in polysorbate 80 for injection.