Determination of residual monomers in poly(lactide-co-epsilon-caprolactone) using gas chromatography
Determination of residual monomers in poly(lactide-co-epsilon-caprolactone) using gas chromatography
复制标题
气相色谱法测定聚丙交酯-ε-己内酯中的残留单体
DOI：
10.1016/j.polymertesting.2020.106998
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发表时间：
2020
期刊：
影响因子：
5.1
通讯作者：
Xuesi Chen
中科院分区：
文献类型：
--
作者：
Lidong Feng;Sheng Xiang;Yanlong Liu;Xinchao Bian;Gao Li;Xuesi Chen
建立了一种用气相色谱内标法定量测定聚（丙交酯-ε-己内酯）（PLCL）中残余单体丙交酯（LA）和ε-己内酯（CL）的分析方法。首先将PLCL和作为内标的二苯醚（DPE）溶解在二氯甲烷（DCM）中，然后将PLCL沉淀在环己烷中。将PLCL中的残留LA和CL单体以及DPE从聚合物溶液中萃取到环己烷中。将所得溶液直接注入GC系统中。该方法可用于PLCL中LA和CL残留量的测定。LA和CL测量的相对标准偏差（RSD）（n= 5）表示该方法的重复性，分别小于5.6%和4.3%，表明该方法具有足够的精密度。PLCL中LA和CL的加标回收率分别为96.5%~ 101.5%和98.4%~ 104.2%。加标回收率的RSD（n= 5）不大于2.0%，表明该方法具有足够的准确度。
An analytical method was developed to quantitatively determine residual monomers, namely, lactide (LA) andε-caprolactone (CL), in poly(lactide-co-ε-caprolactone) (PLCL) using an internal-standard method of gas chromatography (GC). PLCL and diphenyl ether (DPE) as an internal standard were initially dissolved in dichloromethane (DCM), and then PLCL was precipitated in cyclohexane. The residual LA and CL monomers in PLCL, as well as DPE, were extracted into cyclohexane from the polymer solution. The resulting solution was directly injected into a GC system. This method was practical for measuring the residual LA and CL contents in PLCL. The relative standard deviation (RSD) (n= 5) denoting the repeatability of this method was less than 5.6% and 4.3% for the LA and CL measurements, respectively, indicating that the method was sufficiently precise. The recovery rate of standard addition was 96.5%–101.5% and 98.4%–104.2% for the determination of LA and CL in PLCL, respectively. TheRSDof the recovery of standard addition (n= 5) was not more than 2.0%, indicating that the method was sufficiently accurate.