毛细管气相色谱法测定吐温80中氯乙醇、乙二醇、二甘醇的含量

目的: 建立氯乙醇、乙二醇、二甘醇的毛细管气相色谱测定方法,并考察不同厂家吐温80中氯乙醇、乙二醇、二甘醇的含量,为提高吐温80的质量控制标准提供方法及依据。 方法: 采用毛细管气相色谱法,色谱柱为AT-WAX(30 m×0.53 mm×1 μm),进样口温度为230 ℃,检测器温度250 ℃,柱温为120 ℃,保持5 min,以6 ℃·min^-1的升温速度升至200保持2 min,再以40 ℃·min^-1升温至240 ℃,保持19 min,测定吐温80样品中氯乙醇、乙二醇、二甘醇的含量。 结果: 在选定的色谱条件下,3种物质分离良好,氯乙醇的回归方程为Y=189.4X-275.8(r=0.9996),平均回收率为99.6%(n=9),精密度为0.97%(n=6),线性范围为6.2~98.4 μg·mL^-1;乙二醇回归方程为Y=188.5X-323.3(r=0.9997),平均回收率为99.9%(n=9),精密度为1.7%(n=6),线性范围为6.0~80.4 μg·mL^-1;二甘醇回归方程为Y=219.5X-159.3(r=0.9990),平均回收率为99.2%(n=9),精密度为1.6%(n=6),线性范围为6.1~80.1 μg·mL^-1。样品中氯乙醇含量可检出,但均在定量限以下;乙二醇含量为34~42 μg·g^-1;二甘醇含量为13~72 μg·g^-1。 结论: 该方法准确、可靠,可用于吐温80中氯乙醇、乙二醇、二甘醇的检测。同时氯乙醇、乙二醇、二甘醇在不同厂家样品中的含量测定为拟定标准限度提供依据。

Objective: To develop a gas chromatography method for determination of chloroethanol,ethylene glycol and diethylene glycol in Tween 80 and to examine the three impurities mentioned above in Tween 80 obtained from different manufactories. Methods: The analysis of chloroethanol,ethylene glycol and diethylene glycol in Tween 80 was carried out on an AT-WAX capillary gas chromatography column (30 m×0.53 mm×1 μm),the temperature of injection port and detector were 230 ℃ and 250 ℃,respectively.Maintain the temperature of the column at 120 ℃ for 5 minutes,raise the temperature at a rate of 6 ℃·min^-1 to 200 ℃ for 2 minutes,then raise the temperature at a rate of 40 ℃·min^-1 to 240 ℃,and maintain for 19 minutes. Results: A good resolution was obtained by this method between the peaks due to chloroethanol,ethylene glycol and diethylene glycol.The linearity equation of chloroethanol was Y=189.4X-275.8(r=0.9996),the average recovery was 99.6%(n=9),the precision was 0.97%(n=6),and the linear range was 6.2–98.4 μg·mL^-1.The linearity equation of ethylene glycol was Y=188.5X-323.3(r=0.9997),the average recovery was 99.9%(n=9),the precision was 1.7%(n=6),and the linear range was 6.0–80.4 μg·mL^-1.The linearity equation of diethylene glycol was Y=219.5X-159.3(r=0.9990),the average recovery was 99.2%(n=9),the precision was 1.6%(n=6),and the linear range was 6.1–80.1 μg·mL^-1.The contents of chloroethanol in the samples of Tween 80 were all under limit of quatitation,the contents of ethylene glycol in the samples were from 34 to 42 μg·g^-1,and the contents of diethylene glycol were from 13 to 72 μg·g^-1. Conclusion: This method is accurate and precise,which can be applied to examine chloroethanol,ethylene glycol and diethylene glycol.Meanwhile,the results of Tween 80 in different manufactories contribute to setup the limits of chloroethanol,ethylene glycol and diethylene glycol.