目的 为了解决聚乙二醇(M_w≥1 000)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(M_w≥1 000)的高效液相色谱法。方法 采用HPLC测定聚乙二醇(M_w≥1 000)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,5 μm))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4～80 μg·mL^-1内线性关系良好(r＞0.999 0),乙二醇、二甘醇和三甘醇检测限均为25 μg·g^-1,定量限均为100 μg·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(M_w≥1 000)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 (M_w≥1 000), 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, 5 μm) 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 4-80 μg·mL^-1(r＞0.999 0). The limit of detection (LOD) was 25 μg·g^-1, and the limit of quantification (LOQ) was 100 μg·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 (M_w≥1 000).