毛细管气相色谱法测定医用可吸收结扎夹单体乙交酯

Determination of Glycolide Monomer in Medical Absorbable Ligating Clip by Capillaty Gas Chromatography

建立内标-气相色谱法定性定量分析医用可吸收结扎夹中乙交酯单体残留的方法。以六氟异丙醇为溶剂，在磁力搅拌下充分溶解样品。采用HP–5 毛细管柱(30 m×0.32 mm，0.25 μm) 为分离柱，检测器为FID。进样口温度为180℃，检测器温度为300℃；采用程序升温，起始温度为80℃，以10℃／min 升至170℃，保持2 min。在选择的色谱条件下，乙交酯和内标物癸内酯得到良好的分离。乙交酯线性范围为0.03～0.15 mg／mL，线性相关系数r=0.999 1，检出限为0.903 μg／mL。测定结果的相对标准偏差为1.06%(n=6)，加标回收率为92.5%~112.7%。该方法样品前处理简单，重现性好，分离效率高，可作为医用可吸收结扎夹残留乙交酯单体的质量控制方法。

The determination of glycolide monomer in medical absorbable ligating clip by capillaty gas chromatography was established. The sample was dissolved by magnetic stirring,with hexafluoroisopropanol as solvent,HP–5 column (30 m×0.32 mm,0.25 μm) and FID were used. The injector temperature was 180℃ , FID temperature was 300℃ . Column temperature programming: initial temperature was at 80℃ , then increased to 170℃ at 10℃/min for 2 minute. Under the selected chromatographic conditions,glycolide and decalactone could get good separation. The linear range of glycolide was 0.03–0.15 mg/mL, correlation coefficient was 0.999 1, and the detection limit was 0.903 μg/mL. The relative standard deviation of detection results was 1.06%(n=6), standard addition recovery was 92.5%–112.7%. This method is simple in sample tratement,has good reproducibility and high separation efficency, it can be used for mass control of glycolide monomer in medical absorbable ligating clip.