毛细管气相色谱法测定聚桂醇原料中乙二醇、月桂醇、二甘醇的含量

Capillary GC determination of ethylene glycol,lauryl alcohol and diethylene glycol in lauromacrogol

目的:建立聚桂醇原料药中3个有关物质乙二醇、月桂醇和二甘醇的毛细管气相色谱测定方法。方法:采用DB-WAX(30 m×0.32 mm×0.25μm)毛细柱,氢火焰离子检测器(FID),进样口温度230℃,检测器温度250℃,程序升温(起始温度180℃,维持7 min,以15℃.min-1的速率升温至230℃,维持40 min)。结果:在选定的色谱条件下,3个物质分离良好。乙二醇的回归方程为Y=846.8X-1.830(r=0.9993),线性范围为0.004～0.2 mg·mL-1,平均回收率为100.0%(n=9);月桂醇的回归方程为Y=2.694×103X-121.8(r=0.9992),线性范围为0.08～4.0 mg·mL-1,平均回收率为100.7%(n=9);二甘醇的回归方程为Y=1.018×103X-3.010(r=0.9992),线性范围为0.004～0.2 mg·mL-1,平均回收率为99.6%(n=9)。结论:本方法能用于聚桂醇原料的质量检测。

Abstract Objective：To establish a capillary GC method for the determination of ethylene glycol, lauryl alcohol and diethylene glycol in lauromacrogol. Methods： A DB - WAX column （ 30 m × 0. 32 mm× 0. 25 μm） was adopt- ed. The inlet temperature was controlled at 230 ℃ and the FID detector temperature was 250 ℃. The oven tempera- ture was initially held at 180 ℃ for 7 rain and was then programmed to 230 ℃ at 15 ℃. min -1 and held for anoth- er 40 rain. Rcsults：A good resolution was obtained between the peaks of ethylene glycol, lauryl alcohol and diethyl- ene glycol. The linearity equation of ethylene glycol was Y = 846. 8X - 1. 830 （ r = 0. 9993 ） , the linear range was 0. 004 -0. 2 mg.mL-1, and the average recovery was 100.0% （n = 9 ）. The linearity equation of lauryl alcohol was Y =2. 694 × 103X - 121.8（r =0. 9992） ,the linear range was 0. 08 -4.0 mg . mL-1 ,and the average recovery was 100. 7 % （n = 9 ）. The linearity equation of diethylene glycol was Y = 1.018 × 103X -3.010 （r = 0. 9992）, the linear range was 0. 004 -0. 2 mg.mL-1 ,and the average recovery was 99.6% （n =9）. Conclusion：The method can be operated for the lauromacrogol quality control.