药用聚酯瓶中乙醛测定方法分析与优化  

Analysis and optimization of determination method of acetaldehyde in pharmaceutical polyester bottles

作　　者：王丹丹 程磊 俞辉 WANG Dan-dan;CHENG Lei;YU Hui(Zhejiang Institute for Food and Drug Control,Key Laboratory of Drug Contacting Materials Quality Control of Zhejiang Province,Hangzhou 310052,China)

机构地区：[1]浙江省食品药品检验研究院浙江省药品接触材料质量控制研究重点实验室,杭州310052

出　　处：《药物分析杂志》2021年第5期893-898,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：国家药典委员会药品标准修订研究课题-乙醛测定法标准提高(2020Y08)。

摘　　要：目的:分析药用聚酯(PET)瓶中乙醛测定法现状,并对其进行标准提高。方法:采用优化后的HS-GC法测定药用PET瓶中乙醛残留量。顶空平衡温度40℃,定量环温度50℃,传输线温度60℃,对照品顶空平衡时间30 min,样品顶空平衡时间8 h,进样体积1 m L;色谱柱HP-INNOWax(30 m×0.320 mm×0.25μm),柱温50℃,进样口温度200℃,检测器温度250℃,载气氮气,柱流量1.5 m L·min^(-1),分流比30∶1。结果:采用优化后的乙醛测定方法,乙醛对照品进样量在0.2~3.0μg范围内呈良好线性关系,r=0.9996;高、中、低加样回收率分别为98.6%、106.3%和100.4%。优化前后乙醛测定法测得乙醛含量结果无显著性差异。结论:优化提高后的乙醛测定法能快速、准确地测定药用PET瓶中乙醛含量,该研究为乙醛测定法的标准提高以及药用PET瓶的质量控制提供指导意义。Objective:To analyze the current situation of determination of acetaldehyde in pharmaceutical polyester(PET)bottle,and to improve its standard.Methods:The optimized HS-GC method was used to determine acetaldehyde residue in pharmaceutical PET bottles.Headspace equilibrium temperature was 40℃,loop temperature was 50℃,transmission line temperature was 60℃,headspace equilibrium time of reference substance was 30 min,headspace equilibrium time of sample was 8 h,injection volume was 1 mL;column temperature was 50℃,inlet temperature was 200℃,detector temperature was 250℃,carrier gas was nitrogen,column flow rate was 1.5 mL·min^(-1),split ratio was 30∶1.Results:Acetaldehyde has shown good linear relationship within the range of 0.2-3.0μg(r=0.9996).The recoveries of high,medium and low concentrations of adding were 98.6%,106.3%and 100.4%,respectively.There was no significant difference between the results of acetaldehyde content measured by acetaldehyde method before and after optimization.Conclusion:The optimized acetaldehyde determination method can determine the acetaldehyde content in the pharmaceutical PET bottles quickly and accurately.This study provides guidance for the improvement of the standard of acetaldehyde determination method and the quality control of the pharmaceutical PET bottle.

关 键 词：顶空气相色谱法 药用聚酯瓶 乙醛含量 测定 标准提高 

分 类 号：R917[医药卫生—药物分析学]