HPLC-ELSD测定脑硬膜密封系统主要降解产物PEG15000的含量

Determination of the main degradation product of dural sealant system PEG 15000 by HPLC- ELSD

目的： 建立高效液相色谱-蒸发光散射法（HPLC-ELSD）测定脑硬膜密封系统的主要降解产物聚乙二醇（PEG）15000的含量。 方法： 采用Inertex C18色谱柱（150 mm×4.6 mm，5 μm），柱温35 ℃，以甲醇-水为流动相，梯度洗脱，流速1.0 mL·min^-1；ELSD参数：漂移管温度40 ℃，载气流量3.0 L·min^-1，进样量20 μL。 结果： 标准溶液中PEG 15000浓度在0.2-20 mg·mL^-1内线性关系良好（r=0.9995）；最低检测限为0.2 mg·mL^-1。低、中、高浓度批内、批间精密度 RSD均小于6%，方法回收率均在90%-101%之间；稳定性实验中低、中、高浓度在30 d内样本冻融后浓度变化均在±10%以内。 结论： 该法经方法验证可用于PEG 15000的含量测定。

Objective： To establish an HPLC-ELSD method for determination of polyethylene glycol（PEG）15000,a main degradation product of dural sealant system. Methods： The HPLC-ELSD was used with an Inertex C18 column（150 mm×4.6 mm,5 μm）at 35 ℃.The mobile phase composed of a mixture of methanol and water with gradient elution at a flow rate of 1.0 L·min^-1.The ELSD drift tube temperature was set at 40 ℃,the flow of dry air was 3.0 L·min^-1,and the injection volume was 20 μL. Results： The PEG 15000 had a good linear relationship in the range of 0.2-20 mg·mL^-1（r=0.9995）.The limit of detection（LOD）was 0.2 mg·mL^-1.The relative standard deviation（RSD）values of the intra-batch and inter-batch precisions at high,middle and low concentrations were all less than 6%. The RSD of the recovery was between 90 % and 101 %.The variations at high,middle and low concentrations of thawed samples within 30 d were in the range of±10 % in the stability test. Conclusion： This HPLC-ELSD method is in accordance with the requirements of the methodology validation,and could be used for the quality control of PEG 15000.