摘要
目的为了解决聚乙二醇(Mw≥1000)中乙二醇、二甘醇和三甘醇《中国药典》(2015年版)气相色谱法存在的分析时间过长、色谱柱不耐用等问题,建立适合聚乙二醇后增加(Mw≥1000)的高效液相色谱法。方法采用HPLC测定聚乙二醇(Mw≥1000)中乙二醇、二甘醇和三甘醇的含量。色谱条件:采用示差折光检测器(RID),以磺化交联的钾离子交换柱(Sepax Carbomix K-NP5:8%(7.8 mm×300 mm,5μm))为色谱柱,以水为流动相,通过三因素三水平正交实验,确定最优的色谱条件为:流速0.4 min·mL^(-1),检测器温度50℃,柱温75℃。结果方法专属性良好,乙二醇、二甘醇和三甘醇在4~80μg·mL^(-1)内线性关系良好(r>0.9990),乙二醇、二甘醇和三甘醇检测限均为25μg·g^(-1),定量限均为100μg·g^(-1)。结论本实验建立的方法简便易行,准确,专属性强,耐用性好,解决了现行方法分析时间过长、样品易污染系统等问题,可用于聚乙二醇(Mw≥1000)中乙二醇、二甘醇和三甘醇的测定。
OBJECTIVE To develop a high-performance liquid chromatography(HPLC)method for simultaneous determination of ethylene glycol,diethylene glycol and triethylene glycol in polyethylene glycol(Mw≥1000),and solve the problems in the current pharmacopoeia determination methods,such as time consuming and low durability of chromatographic columns.METHODS The detection was performed on a Sepax Carbomix K-NP5:8%column(7.8 mm×300 mm,5μm)with a RID detector.The optimal chromatographic condition was determined by three-factor and three-level orthogonal experiments.The mobile phase consisted of water and was eluted at a flow rate of 0.4 min·mL^(-1)with RID temperature of 50℃and column temperature of 75℃.RESULTS The method was specific.The linearity of each component was excellent in the range of 4-80μg·mL^(-1)(r>0.9990).The limit of detection(LOD)was 25μg·g-1,and the limit of quantification(LOQ)was 100μg·g^(-1).CONCLUSION The method established in this paper is simple,accurate,specific,and durable.It can be used for the determination of ethylene glycol,diethylene glycol and triethylene glycol in polyethylene glycol(Mw≥1000).
作者
周小华
庞文倩
赵恂
陈蕾
邱志霞
张玫
袁耀佐
ZHOU Xiao-hua;PANG Wen-qian;ZHAO Xun;CHEN Lei;QIU Zhi-xia;ZHANG Mei;YUAN Yao-zuo(Jiangsu Institute for Food and Drug Control,Naning 210019,China;China Pharmaceutical Universiry,Naning 210009,Chi na;Chinese Pharmacopoeia Commissio n.Beijing 100061,China)
出处
《中国药学杂志》
CAS
CSCD
北大核心
2021年第8期682-687,共6页
Chinese Pharmaceutical Journal
关键词
高效液相色谱法
聚乙二醇
乙二醇
二甘醇
三甘醇
HPLC
polyethylene glycol
ethylene glycol
diethylene glycol
triethylene glycol
