乙交酯-己内酯共聚物中单体残留量的测定

Determination of Residual Monomer in Glycolide ε-caprolactone Copolymer

建立气相色谱质谱联用法定性定量分析乙交酯-己内酯共聚物中单体残留的方法。以二氯甲烷溶剂,超声萃取样品。采用DB1701毛细管柱(30 m×320μm×0.25μm)为分离柱。进样口温度为180℃;采用程序升温,起始温度为50℃,以10℃/min升至190℃,保持2 min。在选择的色谱条件下,乙交酯和己内酯得到良好的分离。两个单体线性范围为0.5~20μg/mL,线性相关系数为乙交酯0.9996和己内酯0.9983,检出限为乙交酯2.07μg/mL和己内酯1.29μg/mL。测定结果的相对标准偏差为0.6%~0.7%(n=6),加标浓度为5.0μg/mL时,回收率在95.6%~97.8%。该方法样品前处理简单,重现性好,分离效率高,适用于乙交酯-己内酯共聚物残留单体的检测方法。

The determination of residual monomer in glycolide caprolactone copolymer by Gas chromatography-mass spectrometry was established. The sample was extracted by Ultrasonic water bath,with dichloromethane as solvent, DB1701 column（30 m×320 μm, 0.25 μm） was used. The injector temperature was 180 ℃. Column temperature programming： initial temperature was at 50 ℃, and then increased to 180 ℃ at 10 ℃/min for 2 minute. Under the selected chromatographic conditions, glycolide and ε-caprolactone could get good separation. The linear range of glycolide and ε-caprolactone were 0.5-20 μg/mL, correlation coefficient were 0.9996 and 0.9983, and the detection limit were 2.07 μg/mL and 1.29 μg/mL. The relative standard deviation of detection results were 0.6 %-0.7 %（n=6）, standard addition recovery was 95.6 %-97.8 %. This method is simple in sample tratement, has good reproducibility and high separation efficiency. It is suitable for the composition determination in glycolide ε-caprolactone copolymer.