HPLC-CAD法测定壬苯醇醚及壬苯醇醚栓中游离PEG的含量  

Determination of free PEG in nonoxinol and nonoxinol suppositories by HPLC-CAD

作　　者：张伟[1] 张慧[1] 梁成罡[1] ZHANG Wei;ZHANG Hui;LIANG Cheng-gang(National Institutes for Food and Drug Control,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院,北京102629

出　　处：《药物分析杂志》2021年第8期1417-1422,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：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-C_(18)色谱柱(4.6 mm×250 mm,5μm),流动相为甲醇-水(80∶20),流速1.0 mL·min^(-1),柱温35℃,进样量20μL,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0.006μg,定量下限0.01μg,线性范围为1.05~5.25μg·mL^(-1)(r=0.9997),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-C_(18) column(4.6 mm×250 mm,5μm),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 20μL,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 0.006μg,the lower limit of quantification was 0.01μg,and the linear range was 1.05-5.25μg·mL^(-1)(r=0.9997).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.

关 键 词：高效液相色谱法 电喷雾检测器 壬苯醇醚 壬苯醇醚栓 游离聚乙二醇 

分 类 号：R917[医药卫生—药物分析学]