目的:建立顶空气相色谱法测定药用辅料15-羟基硬脂酸聚乙二醇酯中的残留杂质环氧乙烷和二氧六环的含量。为15-羟基硬脂酸聚乙二醇酯的质量控制提供参考和依据。方法:参考国内外药典方法,选用色谱柱DB-5(15 m×0.32 mm, 1μm),以5%苯...目的:建立顶空气相色谱法测定药用辅料15-羟基硬脂酸聚乙二醇酯中的残留杂质环氧乙烷和二氧六环的含量。为15-羟基硬脂酸聚乙二醇酯的质量控制提供参考和依据。方法:参考国内外药典方法,选用色谱柱DB-5(15 m×0.32 mm, 1μm),以5%苯基-95%甲基聚硅氧烷为固定液,采用程序升温模式:起始温度为35℃,维持5 min,以每分钟5℃的速率升温至180℃,然后以每分钟30℃的速率升温至250℃,维持5 min。进样口温度为150℃,检测器温度为250℃,顶空平衡温度70℃,平衡时间45 min,分流比为10∶1。按标准加入法计算供试品中环氧乙烷和二氧六环的含量。结果:在该色谱条件下,环氧乙烷和二氧六环分别在0.5~4μg·mL^(-1)和5~40μg·mL^(-1)范围内线性关系良好(r≥0.99);平均回收率均为75%(RSD=5%,n=9)。来自三个厂家的五批次样品均未检测出环氧乙烷,其中一批样品未检出二氧六环,另外四批样品中二氧六环含量均小于0.005%,符合限度要求。结论:该方法适用于15-羟基硬脂酸聚乙二醇酯中环氧乙烷和二氧六环含量测定,为15-羟基硬脂酸聚乙二醇酯的质量控制提供了参考与指导。展开更多
In order to prepare the polyethylene materials with controlling properties,we developed two kinds of controllable cross-linking polyethylene foaming system.2,5-dimethyl-2,5-bis (tert-butyl peroxy) hexane was used as c...In order to prepare the polyethylene materials with controlling properties,we developed two kinds of controllable cross-linking polyethylene foaming system.2,5-dimethyl-2,5-bis (tert-butyl peroxy) hexane was used as cross-linking agent and TEMPO as cross-linking inhibitor,azodicarbonamide (AC) was used as foaming agent and citric acid as foaming promoter.The density,expansion ratio,cellular structure and mechanical property of these two kinds of controllable materials were studied.Experimental results show that,properties of these two kinds of materials appear similar trend:cellular size and expansion ratio are enlarged with the amount of cross-linking inhibitor or foaming promoter increasing,while density and mechanical strength appear decreasing trend.Through comparing those two material systems’ properties,cross-linking polyethelene foaming system with citric acid as foaming promoter has better properties.展开更多
基金Funded by National Natural Science Foundation of China (No.21975108)Fundamental Research Funds for the Central Universities of China (No.JUSRP121033)。
文摘In order to prepare the polyethylene materials with controlling properties,we developed two kinds of controllable cross-linking polyethylene foaming system.2,5-dimethyl-2,5-bis (tert-butyl peroxy) hexane was used as cross-linking agent and TEMPO as cross-linking inhibitor,azodicarbonamide (AC) was used as foaming agent and citric acid as foaming promoter.The density,expansion ratio,cellular structure and mechanical property of these two kinds of controllable materials were studied.Experimental results show that,properties of these two kinds of materials appear similar trend:cellular size and expansion ratio are enlarged with the amount of cross-linking inhibitor or foaming promoter increasing,while density and mechanical strength appear decreasing trend.Through comparing those two material systems’ properties,cross-linking polyethelene foaming system with citric acid as foaming promoter has better properties.
