目的:研究并建立HPLC-CAD 法测定壬苯醇醚及壬苯醇醚栓中游离聚乙二醇(PEG)的含量。方法:采用HALO ES-C18 色谱柱(4.6 mm×250 mm, 5 μm), 流动相为甲醇- 水(80∶20), 流速1.0 mL·min-1, 柱温35 ℃, 进样量20 μL, 检测器为CAD, 雾化气体为氮气, 蒸发管温度50 ℃, 气流压力约6.895 kPa。结果:PEG 400 的检测下限为0.006 μg, 定量下限0.01 μg, 线性范围为1.05~5.25 μg·mL-1(r=0.999 7), 壬苯醇醚、壬苯醇醚栓的平均回收率(n=3)分别为99.3%~101.6%(RSD=0.10%~0.30%)和103.1%~104.9%(RSD=0.10%~0.20%)。结论:该方法简单、快速、灵敏、准确, 适合对壬苯醇醚及壬苯醇醚栓中游离PEG 进行质量控制。
Objective:To study and establish an HPLC-ELSD (electrospray detector) method for the determination of free PEG in nonoxinol and nonoxinol suppositories. Methods:Free PEG was determined by HPLC-CAD with an HALO ES-C18 column (4.6 mm×250 mm, 5 μm), the mobile phase was methanol-water (80∶20) at the flow rate of 1.0 mL·min-1, the column temperature was 35 ℃ and the injection volume was 20 μL, CAD was used as detector, the evaporate tube temperature was 50 ℃, the nebulizer gas was nitrogen and the flow pressure was around 6.895 kPa. Results:The lower limit of detection for PEG 400 was 0.006 μg, the lower limit of quantification was 0.01 μg, and the linear range was 1.05-5.25 μg·mL-1 (r=0.999 7). The mean recovery (n=3) of nonoxinol and nonoxinol suppositories were 99.3%-101.6% (RSD=0.10%-0.30%) and 103.1%-104.9% (RSD=0.10%-0.20%). Conclusion:This method is simple, fast, sensitive, accurate and suitable for the quality control of free PEG in nonoxinol and nonoxinol suppositories.
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