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《化学分析计量》 2019年第05期
DOI:10.3969/j.issn.1008-6145.2019.05.006
气相色谱法测定可吸收缝线降解产物中的乙醇酸
徐萍华,鲍娇慧,王敏珠,张莉,韩银
浙江省医疗器械检验研究院,杭州 310018 
Determination of glycolic acid in absorbable suture degradation product by gas chromatography
XU Pinghua, BAO Jiaohui, WANG Minzhu, ZHANG Li, HAN Yin
Zhejiang Institute of Medical Device Supervision and Testing, Hangzhou 310018, China 
摘要:采用毛细管气相色谱法测定可吸收缝线降解产物中乙醇酸的含量。选用磷酸二氢钾和磷酸氢二钠混合溶液对可吸收缝线浸提,用甲醇-硫酸溶液对浸提液进行甲酯化反应后进行GC分析。色谱条件:DB-Wax 毛细管柱(30 mm×0.32 mm,0.5 μm),FID检测器;进样口温度为250℃;检测器温度为300℃;柱程序升温,起始温度为70℃,以5℃/min的速度升温至100℃,然后以25℃/min的速度升温至220℃,保持2 min;外标法定量。在选定的色谱条件下,乙醇酸的质量浓度在0.098 1~0.981 0 mg/mL范围内与色谱峰面积呈良好的线性关系,线性相关系数r2=0.999 6,检出限为1.72 μg/mL。测定结果的相对标准偏差为0.67%~1.87%(n=6),加标回收率为97.9%~104.2%。该方法操作简单、快速、稳定,适用于对医用合成可吸收缝线-聚乙交酯的质量控制。 
Abstract:Capillary gas chromatography was used to determine the content of glycolic acid in the degradation products of absorbable suture. The absorbable suture was extracted by using a mixed solution of potassium dihydrogen phosphate and disodium hydrogen phosphate. After the methyl esterification by methanol-sulfuric acid, the extract was subjected to GC analysis, and the feasibility was verified by methodology. The chromatographic conditions were as follows: DB-Wax capillary column (30 mm×0.32 mm, 0.5 μm), FID detector; inlet temperature was 250℃; detector temperature was 300℃; column temperature programmed, starting temperature was 70℃, heat up to 100℃at 5℃/min, then heat up to 220℃at 25℃/min kept for 2 min. The external standard method was used for quantification. Under the selected chromatographic conditions, the mass concentration of glycolic acid has a good linear relationship with the chromatographic peak area in the range of 0.098 1-0.981 0 mg/mL (r2=0.999 6), the detection limit was 1.72 μg/mL. The relative standard deviation of determination results was 0.67-1.87%(n=6) and the recoveries were 97.9%-104.2%. The method is simple, rapid and stable, which is suitable for quality control of medical synthetic absorbable suture-polyglycollide. 
关键词:乙醇酸;甲酯化;气相色谱法;可吸收缝线 
Keywords:glycolic acid; methyl esterification; gas chromatography; absorbable suture 
基金:浙江省科技厅省属科研院所扶持专项(2017F50026) 
本文引用格式:
徐萍华,鲍娇慧,王敏珠,等.气相色谱法测定可吸收缝线降解产物中的乙醇酸[J].化学分析计量,2019,28(5):24-28. XU P H,BAO J H,WANG M Z,et al. Determination of glycolic acid in absorbable suture degradation product by gas chromatography[J]. Chemical analysis and meterage,2019,28(5):24-28. 

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