HPLC/ELSD测定聚山梨酯80中聚醚组成及油酸含量

目的: 建立聚山梨酯80中聚醚组成及油酸含量的高效液相色谱测定方法,并考察不同厂家聚山梨酯80中聚醚组成及油酸含量;为提高聚山梨酯80的质量控制标准提供方法及依据。 方法: 采用液相色谱法,色谱柱为Waters Xbridge^TM Amide柱(150 mm×4.6 mm,3.5 μm),柱温为30 ℃,流速0.5 mL·min^-1;蒸发光散射检测器,漂移管温度55 ℃,N₂流速1.6 L·min^-1。测定聚山梨酯80样品中聚醚组成及油酸含量。 结果: 在选定的色谱条件下,4种物质分离良好,油酸的回归方程为lnY=1.883lnX+7.037(r=0.9998),平均回收率为101.4%(n=9), 线性范围为9.936~99.36 μg·mL^-1;异山梨醇聚醚的回归方程为lnY=1.467lnX+8.456(r=0.9988),平均回收率为101.2%(n=9),线性范围为8.656~86.56 μg·mL^-1;一失水山梨醇聚醚的回归方程为lnY=1.482lnX+8.336(r=0.9998),平均回收率为104.8%(n=9),线性范围为23.02~230.2 μg·mL^-1;山梨醇聚醚的回归方程为lnY=1.159lnX+9.202(r=0.9974),平均回收率为95.4%(n=9),线性范围为4.604~46.04 μg·mL^-1。不同来源的样品其聚醚组成及油酸有较大的差异。 结论: 该方法准确、可靠,可用于聚山梨酯80中聚醚组成及油酸含量的检测。同时为不同厂家样品中聚醚组成及油酸的含量拟定标准限度提供依据。

Objective: To establish a liquid chromatography method for the content determination of oleic acid,polyoxyethylene isosorbide,polyoxyethylene sorbitan and polyoxyethylene sorbitol in polysorbate 80,and examine the four chemical compositions in polysorbate 80 from different manufactories,so as to provide a basis for the improvement of polysorbate 80 quality control standards. Methods: The analysis was carried out on a Waters Xbridge^TM Amide liquid chromatography column(150 mm×4.6 mm,3.5 μm)with the column temperature at 30 ℃ and mobile phase at a flow rate of 0.5mL·min^-1;ELSD was operated under following conditions:drift tube temperature was 75 ℃ and N₂ flow was 1.6 L·min^-1. Results: A good resolution was obtained by this method between the peaks of oleic acid,polyoxyethylene isosorbide,polyoxyethylene sorbitan and polyoxyethylene sorbitol.The linearity equation of oleic acid was lnY=1.883×lnX+7.037(r=0.9998),the average recovery was 101.4%(n=9)and the linear range was 9.936~99.36 μg·mL^-1.The linearity equation of polyoxyethylene isosorbide was lnY=1.467lnX+8.456(r=0.9988),the average recovery was 101.2%(n=9)and the linear range was 8.656-86.56 μg·mL^-1.The linearity equation of polyoxyethylene sorbitan was InY=1.482InX+8.336(r=0.9998),the average recovery was 104.8%(n=9)and the linear range was 23.02-230.2 μg·mL^-1.The linearity equation of polyoxyethylene sorbitol was InY=1.159InX+9.202(r=0.9974),the average recovery was 95.4%(n=9)and the linear range was 4.604-46.04 μg·mL^-1.The results also showed that the components of polyether and oleic acid are very different among polysorbate 80 from different manufacturers. Conclusion: This method is accurate and precise, which can be applied to the examination of oleic acid,polyoxyethylene isosorbide,polyoxyethylene sorbitan and polyoxyethylene sorbitol. Meanwhile, the results of polysorbate 80 in different manufactories contribute to establishment of standard limits of oleic acid,polyoxyethylene isosorbide,polyoxyethylene sorbitan and polyoxyethylene sorbitol.