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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,5μm),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20μL。结果:标准溶液中PEG 15000浓度在0.2~20mg·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 a HPLC-ELSD method for the determination of polyethylene glycol (PEG) 15000, a major degradation product of the brain dura mater. Methods: Inertex C18 column (150 mm × 4.6 mm, 5 μm) was used. The column temperature was 35 ℃ and the mobile phase consisted of methanol and water with a gradient of 1.0 mL · min-1. The ELSD parameters were as follows: , Carrier gas flow 3.0 L · min-1, injection volume 20μL. Results: The linearity of PEG 15000 in standard solution was 0.2 ~ 20 mg · mL-1 (r = 0.9995). The lowest detection limit was 0.2 mg · mL-1. RSD of intra-batch and inter-batch precision of low, medium and high concentrations were less than 6%, and the recovery rates of methods were all between 90% and 101%. After freeze-thaw cycles of low, middle and high concentration samples in 30 days Concentration changes are within ± 10%. Conclusion: This method is validated by the method of PEG 15000 content determination.