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 C18色谱柱(100 mm×2.1 mm,1.7 μm),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0.1～10.5 μg·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0.02～2.0 μg·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0.02 μg·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 C18 column(100 mm×2.1 mm, 1.8 μm)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 0.1-10.5 μg·mL-1(r=1.000), and PBT tetramer and PBT pentamer showed a good linear relationship in the range of 0.02-2.0 μg·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 0.02 μg·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.
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