高效液相色谱法检测溴化丁基胶塞中11种抗氧剂及游离硫的浸出量及迁移量

采用Inertsil ODS-SP C18(250×4.6 mm,5μm)色谱柱,以0.1%乙酸水-甲醇-乙腈为流动相,进行梯度洗脱,流速为1.0 mL/min,检测波长为277 nm。胶塞提取溶剂分别为无水乙醇和模拟药液。11种抗氧剂及游离硫的分离度均大于1.5;在2.47~54.51μg/mL浓度范围内,线性关系良好(R^2均大于0.999);检出限为0.021~0.403μg/mL;以无水乙醇为提取溶剂时,加标回收率为82.8%~115.3%,相对标准偏差为1.1%~6.1%;以模拟药液为提取溶剂时,加标回收率为62.9%~103.2%,相对标准偏差为1.4%~5.6%。该方法可用于包材相容性试验中实际样品的检测。

Leaching and migration studies on 11 antioxidants and free sulfur in brominated butyl rubber plugs

The extraction solvents were anhydrous ethanol and drug simulant,and the results showed that the separation degree of 11 kinds of antioxidants and free sulfur was greater than 1.5-fold by using Inertsil ODS-SP C18(250×4.6 mm,5μm)column at the detection wavelength of 277 nm with 0.1%acetic acid-watermethanol-acetonitrile that utilized as the mobile phase in gradient elution model.The flow was set as1.0 m L/min.11 kinds of antioxidants and free sulfur presented good linear relationship in the range of 2.47~54.51μg/m L(R^2>0.999).The limit detections were 0.021~0.403μg/m L.When using anhydrous ethanol as extraction solvent,the recoveries were between 82.8%and 115.3%with the relative standard deviations between 1.1%and 6.1%.When the drug simulant was used as the extraction solvent,the recoveries were between 62.9%and 103.2%with the relative standard deviations between 1.4%and 5.6%.The method can be used to detect the actual samples in the compatibility test of packing materials.