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

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

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。

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.