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Title:: Study on the Residual Endcapper in Biodegradable Poly( lactic acid )

作者:: 刘阳1; 2; 马丽霞2; 王勤2 ; 王传栋2△; 冯圣玉1; 1.山东大学化学与化工学院,济南 250100;2.山东省药学科学院，山东省生物医用高分子材料重点实验室，济南 250101

Author(s):: LIU Yang1; 2; MA Lixia2; WANG Qin2; WANG Chuandong2; FENG Shengyu1; 1.Institute of Chemistry and Chemical Technology，Shandong University，Jinan 250100，China；2.Shandong Academy of Pharmaceutical Sciences,Shandong Provincial Key Laboratory of Biomedical Polymers, Jinan 250101

Keywords:: Poly ( lactic acid ); Endcapper; gas chromatography ( GC ); Hydrogen flame ionization detector ( FID )

摘要:: 建立了一种气相色谱法测定聚乳酸原料中封端剂十二醇残留的分析方法。着重研究了测定方法及样品的预处理方法。实验结果显示，采用DB-624（30m×0.530mm×3.0μm）毛细管柱，氢火焰离子检测器，进样口温度250℃，检测器温度260℃，程序升温（起始温度60℃，维持3 min，以30℃/min的速率升温至250℃，维持10min），十二醇的回归方程为A=2717.3C -11.646（γ=0.9998），线性范围为0.01～1.01 mg/mL，平均回收率为99.21%（n=9），相对标准偏差1.55%，检测限为0.0005 mg/mL，定量限为0.001 mg/mL。本实验所建立的方法能达到定量检测的目的，将该方法应用于聚乳酸原料中封端剂十二醇残留量的测定，结果可靠。

Abstract:: A gas chromatography method was developed for the determination of lauryl alcohol residual in poly ( lactic acid ). It focused on studying the gas chromatography method and the pretreatment method of PLA. The result of the experiment showed that a DB-624 column (30m×0.53mm×3.0μm) was adopted, the inlet temperature was controlled at 250 ℃ and the FID detector temperature was 260 ℃, the oven temperature was initially held at 60 ℃ for 3 min and was then programmed to 250 ℃ at 30 ℃/min and held for another 10 min, the linearity equation of lauryl alcohol was A=2717.3C-11.646 (γ=0.9998), the linear range was 0.01mg/mL～1.01mg/mL, and the average recovery was 99.21% (n=9), the RSD was 1.55%, the limit of detection was 0.0005mg/mL.The limit of quantification was 0.001mg/mL, the method can achieve the purpose of lauryl alcohol quantitative detection. The analysis of lauryl alcohol residual in poly (lactic acid) verify the reliability of this method.