顶空-气相色谱法测定新型氨基多羧酸型螯合剂中的3种残留溶剂

Determination of the three residual solvents in a novel aminopolycarboxylic acid chelating agent by headspace-gas chromatography

目的 建立顶空-气相色谱法,测定新型氨基多羧酸型螯合剂中的乙醇、乙腈和吡啶3种残留溶剂。方法采用顶空-气相色谱内标法定量。用DB-WAX石英毛细管柱(30 m×0.45 mm,0.85μm)和氢火焰离子化检测器进行分离和检测,载气为高纯氮,程序升温。进样口温度200℃,检测器温度250℃。顶空平衡温度110℃,顶空平衡时间40 min。结果 该方法对乙醇、乙腈和吡啶分离度良好,在相应浓度范围内线性关系良好(r>0.999)。3种残留溶剂的加样回收率分别为100.2%、97.6%和99.4%,检测限为0.08-0.33μg/ml,定量限为0.40-1.33μg/ml。结论 所建立的气相色谱法可用于测定该螯合剂中的3种残留溶剂。

Objective To determine the three residual solvents—ethanol,acetonitrile and pyridine in a new aminopolycarboxylic acid chelating agent using headspace-gas chromatography. Methods Headspace-gas chromatography combined with internal standard method was used for quantification. The samples were separated and detected by DB-WAX capillary column with an flame ionization detector(FID)detector. The carrier gas was high purity nitrogen and the column temperature was programmed. The inlet temperature was 200℃ and the detector temperature was 250℃. The headspace equilibrium temperature was 110℃,and the headspace equilibrium duration was 40 min. Results Ethanol,acetonitrile and pyridine were well separated using this method,and the linear relationship was good in the corresponding concentration range. The recoveries of the three residual solvents were 100.2%,97.6% and 99.4%,respectively,and the detection limit was 0.08-0.33 μg/ml,while the limit of quantification was 0.40-1.33 μg/ml. Conclusion This method can be used to determine the three residual solvents—ethanol,acetonitrile and pyridine in the chelating agent.