高效液相色谱法测定不同硫化体系药用胶塞中的硫化剂及促进剂  

Determination of vulcanizing agents and accelerators in pharmaceutical rubber stoppers with different vulcanization systems by HPLC

作　　者：辜倩 汪元亮 熊马剑 左军凤 朱碧君 GU Qian;WANG Yuan-liang;XIONG Ma-jian;ZUO Jun-feng;ZHU Bi-jun(Jiangxi Institute of Drug Inspection and Testing,Key Laboratory for Quality Evaluation of Chinese Patent Medicines,State Drug Administration,Jiangxi Pharmaceutical and Medical Device Quality Engineering Technology Research Center,Nanchang 330029,China;Jiangxi University of Traditional Chinese Medicine,Nanchang 330004,China)

机构地区：[1]江西省药品检验检测研究院、国家药品监督管理局中成药质量评价重点实验室、江西省药品与医疗器械质量工程技术研究中心,南昌330029 [2]江西中医药大学,南昌330004

出　　处：《药物分析杂志》2023年第2期305-313,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：国家药典委标准提高项目(编号:2019Y03);江西省药品监督管理局科研项目(编号:2021KY13);江西省药品监督管理局科研项目(编号:2019JS04)。

摘　　要：目的:建立HPLC法测定不同硫化体系橡胶塞中硫化剂和促进剂的含量。方法:采用Waters SunFire C18(250 mm×4.6 mm,5μm)色谱柱,以甲醇-水为流动相,进行梯度洗脱,流速1.0 mL·min^(-1),柱温35℃,检测波长220 nm,进样体积10μL,外标法定量。结果:14种成分在不同的浓度范围(0.10~20、0.50~20、1.0~20μg·mL^(-1))内线性关系良好(r=0.9959~1.000);方法的精密度、重复性均小于2.0%,供试品溶液在48 h内稳定。不同硫化体系样品的平均回收率为90.0%~108.7%,RSD(n=6)为0.10%~2.8%。从试验结果来看,胶塞中S普遍存在,含量在0.0030~0.2114 mg·g^(-1)之间,可见硫磺体系目前仍是主要的硫化体系;3批胶塞中检测出N-环己基-2-苯并噻唑次磺酰胺(CZ)(0.0708、0.1443、0.4312 mg·g^(-1)),1批胶塞中检测出一硫化四甲基秋兰姆(TMTM)(0.0991 mg·g^(-1)),表明秋兰姆类等会产生有害物质的促进剂几乎无添加。结论:本方法操作简单,具有较好的精密度和回收率,适用于不同硫化体系硫化剂和促进剂的含量测定,可为胶塞的安全性检测提供参考。Objective:To establish an HPLC method for the determination of vulcanizing agents and accelerators in rubber stoppers with different vulcanization systems.Methods:The chromatographic column of Waters Sunfire C18column(250 mm×4.6 mm,5μm)was gradient eluted with methanol aqueous solution as the mobile phase.The flow rate was 1.0 mL·min^(-1),the column temperature was 35℃,the detection wavelength was set at220 nm,and the injection volume was 10μL.External standard method was used.Results:The the linear relationship was good(r=0.9959~1.000)in different concentration ranges(0.10-20μg·mL^(-1),0.50-20μg·mL^(-1),1.0-20μg·mL^(-1))for 14 components.The precision and repeatability of the method were less than 2.0%,and the test solution was stable within 48 h.The average recovery of rubber stopper samples with different vulcanization systems was 90.0%-108.7%,and the RSD(n=6)was 0.10%-2.8%.The test results showed that free sulfur was prevalent in the stoppers,and the sulfur system was still the main system in the vulcanization of the stoppers.Thiuram harmful accelerators were hardly added.Conclusion:The method is simple to operate,with good precision and recovery.It is suitable for the determination of vulcanizing agent and accelerator with different vulcanization systems,and can provide reference for the safety detection of rubber stopper.

关 键 词：高效液相色谱 药用胶塞 硫化体系 硫化剂 促进剂 含量测定 

分 类 号：R917[医药卫生—药物分析学]