UPLC法测定布地奈德吸入气雾剂中PBT低聚物的迁移量

Determination of PBT oligomers migration in budesonide aerosol by UPLC

目的:建立超高效液相色谱(UPLC)法测定布地奈德吸入气雾剂中聚对苯二甲酸丁二醇酯(PBT)低聚物迁移量。方法:采用ACQUITY BEH C_(18)色谱柱(100 mm×2.1 mm,1.7μm),以水(A)-乙腈(B)为流动相,梯度洗脱,流速0.4 mL·min^(-1),检测波长240 nm。结果:PBT二聚物和PBT三聚物在0.1~10.5μg·mL^(-1)浓度范围内线性关系良好(r=1.000),PBT四聚物和PBT五聚物在0.02~2.0μg·mL^(-1)浓度范围内线性关系良好(r=1.000);各成分的平均加样回收率在94.18%~104.7%(n=6);各成分的检测限均小于0.02μg·mL^(-1)。在布地奈德吸入气雾剂的药液中,不同程度地检出了PBT二聚体和PBT三聚体,但均未检出PBT四聚体和PBT五聚体。结论:该方法准确可靠,选择性好,简便快速,可用于PBT低聚物迁移量的测定及气雾剂包材质量评价。

Objective:To establish a method for the determination of polybutylene terephthalate(PBT)oligomers migration in budesonide aerosol by ultra high performance liquid chromatography(UPLC).Methods:The analysis was performed on an ACQUITY BEH C_(18)column(100 mm×2.1 mm,1.8μm)at 35℃.The mobile phase of water(A)and acetonitrile(B)was subjected to gradient elution(0-1.5 min,40%A→25%A;1.5-8 min,25%A;8-9 min,25%A→10%A;9-12 min,10%A;12-13 min,10%A→40%A;13-16 min,40%A)at a flow rate of 0.4 mL·min^(-1).And the detection wavelength was 240 nm.Results:PBT dimer and PBT trimer showed a good linear relationship in the range of 0.1-10.5μg·mL^(-1)(r=1.000),and PBT tetramer and PBT pentamer showed a good linear relationship in the range of 0.02-2.0μg·mL^(-1)(r=1.000);the average recoveries of the four compounds were 94.2%-104.7%;the detection limits of the four compounds were all less than 0.02μg·mL^(-1).In the solutions of budesonide aerosol,the migration of PBT dimer and PBT trimer were detected in different degrees,but PBT tetramer or PBT pentamer was not found.Conclusion:The method is accurate,reliable,selective,simpleand rapid.It can be used for the determination of PBT oligomers migration and the quality evaluation of aerosol packing materials.