药用丁基胶塞中抗氧剂——BHT和硫化剂——可提取硫的测定  

Determination of antioxidant——BHT and vulcanizing agent——extractable sulphur in medicinal butyl rubber

作　　者：冯靖[1] 蔡心怡[1] 刘言[1] FENG Jing CAI Xin-yi LIU Yan(Tianjin Institute for Drug Control, Tianjin 300070, Chin)

机构地区：[1]天津市药品检验所,天津300070

出　　处：《药物分析杂志》2017年第4期702-706,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立药用丁基橡胶塞中添加剂[抗氧剂264(2,6-二叔丁基-4-甲基苯酚,简称BHT)和硫化剂可提取硫]的含量测定方法。方法:以二氯甲烷-无水乙醇为提取溶剂,利用高效液相色谱法对药用丁基橡胶塞的BHT和可提取硫含量进行测定,以含0.1%三氟乙酸的乙腈-含0.1%三氟乙酸的水(90∶10)为流动相,流速1.0 m L·min^(-1),检测波长280 nm。结果:抗氧剂BHT的线性检测范围0.41~103.00μg·mL^(-1)(r^2=1.000),可提取硫的线性检测范围0.10~103.50μg·mL^(-1)(r^2=0.999 9),BHT和可提取硫的平均回收率分别为95.2%和86.8%。测定7批药用胶塞中BHT与可提取硫含量范围分别为4~206μg·g^(-1)和1~143μg·g^(-1)。结论:本文建立的检测方法经方法学验证,可用于考察药用丁基橡胶塞中BHT和可提取硫的含量及质量控制。Objective： To establish a method for determination of the additives [ antioxidant 264 （ 2, 6-di-tertbutyl-4-methylphenol, hereinafter referred to as BHT ） and vulcanizing agent （ extractable sulphur ） ] in medicinal butyl rubber. Methods： Dichloromethane-ethanol was adopted as the extraction solvent, and the HPLC was used for determination of BHT and extractable sulphur in medicinal butyl rubber. The mobile phase consisted of acetonitrile- water （ 90： 10, containing 0. 1%TFA ）. The flow rate was 1.0 mL· min^-1. The detection wavelength was 280 nm. Results： The linearity ranges wer from 0. 41 to 103.00 μg· mL^-1 （ 2=1. 000 ） and 0. 10 to 103.50μg· mL^-1 （ 2= 0. 999 9 ）for BHT and extractable sulphur. The average recoveries of BHT and extractable sulphur were 95.2% and 86.8%, respectively. The determination results of BHT and extractable sulphur sulphur in seven batch rubbers were 4-206 μg · g^-1 and 1-143 μg · g^-1 respectively. Conclusion： The validated method established in this article can be used for the assay of BHT and extractable sulphur content and for its quality control in medicinal butyl rubber.

关 键 词：药品包装容器 丁基胶塞 抗氧剂 硫化剂 2 6-二叔丁基-4-甲基苯酚(BHT) 可提取硫 高效液相色谱 安全监测 

分 类 号：R917[医药卫生—药物分析学]