HPLC-CAD法同时测定聚乙二醇及壬苯醇醚的含量  

Simultaneous determination of polyethylene glycol and nonoxinol by HPLC-CAD

作　　者：张伟[1] 孙悦[1] 张慧[1] 梁成罡[1] ZHANG Wei;SUN Yue;ZHANG Hui;LIANG Cheng-gang(Division of Hormone,National Institutes for Food and Drug Control,NMPA Key Laboratory for Quality Research and Evaluation of Chemical Drugs,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院激素室,国家药品监督管理局化学药品质量研究与评价重点实验室,北京102629

出　　处：《中国新药杂志》2022年第18期1853-1857,共5页Chinese Journal of New Drugs

摘　　要：目的:建立HPLC-电喷雾检测器(CAD)法同时测定聚乙二醇(PEG)及壬苯醇醚的含量。方法:采用HALO ES-C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-水体系,线性梯度洗脱,流速1.0 mL·min^(-1),柱温35℃,进样量10μL;检测器为CAD,雾化气体为氮气,蒸发管温度50℃,气流压力约60 psi。结果:PEG400的检测限为0.006μg,定量限为0.01μg,线性范围为0.50~1.51 mg·mL^(-1)(r=0.9999),平均回收率为100.8%(n=3,RSD=0.39%);壬苯醇醚的检测限为0.11μg,定量限为1.10μg,线性范围为0.50~3.00 mg·mL^(-1)(r=0.9998),平均回收率为100.8%(n=3,RSD=0.40%)。结论:该方法简单、快速、灵敏、准确,能够同时对PEG及壬苯醇醚进行质量控制。Objective: To establish an HPLC-CAD method for simultaneous determination of polyethylene glycol(PEG)and nonoxinol. Methods: PEG and nonoxinol were determined on an HALO ES-C_(18) column(250 mm×4.6 mm, 5 μm), the mobile phase was methanol-water system, linear gradient elution was performed at the flow rate of 1.0 mL·min^(-1), the column temperature was 35 ℃, and the injection volume was 10 μL. CAD was used as detector, the evaporate tube temperature was 50 ℃, the nebulizer gas was nitrogen, and the flow pressure was around 60 psi. Results: For PEG400, the LOD was 0.006 μg, the LOQ was 0.01 μg, the calibration curves showed good linearity in the range of 0.50~1.51 mg·mL^(-1)(r=0.999 9), and the average recovery was 100.8%(RSD=0.39%, n=3). For nonoxynol, the LOD was 0.11 μg, the LOQ was 1.10 μg, the linearity was in the range of 0.50~3.00 mg·mL^(-1)(r=0.999 8), and the average recovery was 100.8%(RSD=0.40%, n=3). Conclusion: This method is simple, rapid, sensitive, accurate, and suitable for the simultaneous quality control of PEG and nonoxinol.

关 键 词：HPLC法 电喷雾检测器 聚乙二醇 壬苯醇醚 

分 类 号：R917[医药卫生—药物分析学]