【摘要】 建立一种气相色谱–质谱法测定生物降解产品中聚乳酸和聚对苯二甲酸/己二酸/丁二酯2种聚酯材料的方法。利用酯交换反应在高温高压条件下将聚酯材料转变成酯类小分子，通过气相色谱–质谱(GC–MS)仪定量分析酯交换溶液中小分子含量，并计算聚酯材料的准确含量。样品量为0.01～0.1 g，反应温度为220 ℃，反应时间为3 h，反应溶液稀释后用DB–WAX型色谱柱分离，选择离子监测/全扫描(SIM/SCAN)模式，气相色谱–质谱法测定。3种聚酯材料的质量浓度在1～20 mg/L范围内与其各自的色谱峰面积线性关系良好，相关系数均大于0.999，检出限为0.12～0.13 mg/L。聚乳酸样品中PLA的平均含量为98.3%，测定结果的相对标准偏差为1.84%，聚对苯二甲酸/己二酸/丁二酯中PBAT的平均含量为101.0%，测定结果的相对标准偏差为1.47%(n=6)。使用市售的聚乳酸、聚己内酯、聚丁二酸丁二醇酯、聚丁二酸-己二酸丁二酯塑料粒子对该方法进行验证，4种材质样品的实测含量为98.1%～100.6%，与理论值偏差较小。更多还原

【Abstract】 A method for the determination of 2 polyester materials in biodegradable products by gas chromatography–mass spectrometry was established,including polylactic acid and polyterephthalic acid / adipic acid / butylene glycol.The polyester materials were transformed into ester small molecules by transesterification reaction under high temperature and high pressure.The content of small molecules in the transesterification solution was quantitatively analyzed by gas chromatography–mass spectrometry(GC–MS),and the accurate content of polyester material was calculated.The sample amount was 0.01–0.1 g,the reaction temperature was 220 ℃,and the reaction time was 3 h.After the reaction solution was diluted,it was separated by DB–WAX chromatographic column,the ion monitoring/full scanning mode was selected,and determined by gas chromatography-mass spectrometry The mass concentrations of 2 polyester materials had a good linear relationships with their chromatographic peak areas in the range of 1–20 mg/L,respectively，the correlation coefficients were greater than 0.999,and the detection limit was 0.12–0.13 mg/L.The average content of PLA in polylactic acid sample was 98.3%,the relative standard deviation of the determination result was 1.84%(n=6),the average content of PBAT in polyterephthalic acid/ adipic acid/ succinate was 101.0%,and the relative standard deviation of the determination result was 1.47%(n=6).The method was verified by using commercially available PLA,PCL,PBS and PBSA plastic particles.The measured content of the four materials was 98.1%–100.6%,which had little deviation from the theoretical value.更多还原