药用卤化丁基胶塞中硫化剂及抗氧剂的HPLC法测定

Determination of Vulcanizing Agent and Antioxidant in Halogenated Butyl Rubber Stoppers by HPLC

建立了高效液相色谱法同时测定卤化丁基胶塞及其提取物和浸出物中硫化剂对叔辛基苯酚(PTOP)及抗氧剂2,6-二叔丁基-4-甲基苯酚(BHT)。采用Agilent SB-C18色谱柱,以不同比例乙腈和水为流动相,梯度洗脱,检测波长278 nm。PTOP及BHT在5~50μg/ml范围内线性关系良好;提取试验及迁移试验中2种物质的回收率均在80%~120%范围内。卤化丁基胶塞中可提取出一定量的PTOP及BHT,加速及长期放置的药物中,除加速放置24个月的药物中可检出PTOP外,其余样品中均未检出PTOP及BHT。本方法准确、有效,可用于测定药用卤化丁基胶塞中PTOP及BHT的含量及其在药物中的迁移情况。

An HPLC method was established for simultaneous determination of vulcanizing agent p-tertoctylphenol(PTOP)and antioxidant 2,6-di-t-butyl-4-methylphenol(BHT)in halogenated butyl rubber stoppers and their extractables and leachables.An Agilent SB-C_(18) column was used with the mobile phase comprising of different ratios of acetonitrile to water in gradient elution mode.The detection wavelength was set at 278 nm.Both PTOP and BHT had good linearities in the range of 5-50μg/ml.In extraction and migration experiments,the recovery rates of two substances were in the range of 80%-120%.Both PTOP and BHT were extracted from the halogenated butyl rubber stoppers,and they had not been detected in the medicines stored under the accelerate condition for 0,3 and 6 months or under longterm stability storage condition for 10 months.However,PTOP was detected in the medicines stored under the accelerate condition for for 24 months.This method is accurate and suitable for determination of PTOP and BHT in halogenated butyl rubber stoppers for pharmaceutical use and evaluation of the migration situation in medicines.