HPLC法测定药用胶塞中常用抗氧剂及可提取硫向丙泊酚中/长链脂肪乳注射液中的迁移

Determination of migration of common antioxidants and extractable sulfur in medical rubber stoppers to propofol medium/long chain fat emulsion injection by HPLC

目的:建立一种高效液相色谱方法(HPLC),用于考察药用胶塞中常用抗氧剂及可提取硫的提取情况,以及药用胶塞中抗氧剂及可提取硫向丙泊酚中/长链脂肪乳注射液的迁移情况。方法:采用Waters Symmetry RP18(250 mm×4.6 mm, 5μm)色谱柱,流动相为甲醇-乙腈^(-1)%醋酸水溶液,梯度洗脱,检测波长为277 nm,流速为1 mL·min^(-1),柱温为35℃。结果:各组分分离度良好;在0.1~20μg·mL^(-1)范围内线性关系良好,r≥0.999 6;该方法的精密度、稳定性、重复性均良好,RSD均<5.0%;回收率为93.3%~108.7%,RSD为1.8%~12.5%。检出3批药液中均有抗氧剂BHT的迁移,且含量高于其相应人每日允许最大暴露量(PDE)值,有较大安全性风险。结论:该方法具有较高的灵敏度,操作简便,能够用于检测丙泊酚中/长链脂肪乳注射液中抗氧剂的迁移。

Objective:To establish a high-performance liquid chromatography(HPLC)method for investigating the extraction of common antioxidants and extractable sulfur in medical rubber stoppers and the migration of antiox⁃idants and extractable sulfur to propofol medium/long chain fat emulsion injection.Methods:Waters Symmetry RP 18(250 mm×4.6 mm,5μm)was used as chromatographic column with methanol-acetonitrile-1%acetic acid solution as the mobile phase.Detection wavelength,velocity of flow and column temperature were set to 277 nm,1 mL·min^(-1) and 35℃.Results:Good resolution and linear relationship(r≥0.9996)in the range of 0.1-20μg·mL^(-1) were achieved.This method possesses superior precision,stability,repeatability,and all RSD were less than 5%.The rate of recovery was 93.3%-108.7%,and the RSD was 1.8%-12.5%.The migration of antioxidant BHT was detected in three batches of solution and the content was higher than its corre⁃sponding permitted daily exposure(PDE)value,which means there is a large safetyrisk.Conclusion:The meth⁃od represents high sensitivity and is easy to operate,which can effectively detect the migration of antioxidants in propofol medium/long chain fat emulsion injection.