HPLC法测定注射用冷冻干燥用卤化丁基橡胶塞中抗氧剂1010及硫化剂在药液中的迁移

Determination of Antioxidant 1010 and Curing Agent in Halogenated Butyl Rubber Plug for Freeze Drying Injection and Their Migration in Medicines by High Performance Liquid Chromatography

目的:建立HPLC方法,考察药用卤化丁基橡胶塞中的抗氧剂、硫化剂及其在药液中的迁移情况。方法:采用Sunfire-C18(4.6 mm×150 mm,5μm)色谱柱;流动相:乙腈-四氢呋喃-水(6∶3∶1);流速:1.5 mL·min^(-1);检测波长:280 nm;柱温:35℃;进样量:20μL。结果:抗氧剂1010及硫化剂硫磺在浓度0.004～0.5 mg·mL^(-1)具有良好的线性关系(r≥0.9996)。抗氧化剂1010及硫化剂硫磺提取试验回收率范围分别是102.05%～111.55%及91.75%～94.83%;抗氧化剂1010及硫化剂硫磺迁移试验回收率范围分别为98.92%～110.70%及98.68%～106.63%;各回收率试验RSD均不大于5%(n=9)。结论:本方法灵敏、准确、可靠,可用于药用卤化丁基橡胶塞中抗氧剂及硫化剂的提取及迁移研究。

Objective: To establish a HPLC method for determination of antioxidants and curing agents in halogenated butyl rubber plug and their migration in medicine. Methods: A Sunfire-C18 column(4.6 mm×150 mm, 5 μm) was used with acetonitrile-tetrahydrofuran-water(6∶3∶1) as mobile phase. The flow rate was 1.5 mL·min^-1 and the detection wavelength was 280 nm. The chromatography was conducted at 35℃ and 20 μL were injected. Results: Antioxidant 1010 and curing agent sulfur had a good linear relationship(r≥0.9996) in the range of 0.004-0.5 mg·mL^-1. The recovery range of antioxidant 1010 extraction test was 102.05%-111.55%, the recovery range of curing agent sulfur extraction test was 91.75%-94.83%, the recovery range of antioxidant 1010 migration test was 98.92%-110.70%, and the recovery range of curing agent sulfur migration test was 98.68%-106.63%. The RSD of each recovery test was no more than 5%(n=9). Conclusion: The method is sensitive,accurate and reliable, which is suitable for the extraction and migration studies of antioxidants and curing agents in halogenated butyl rubber plug for medicines.