摘要
建立了气相色谱-质谱法测定聚偏二氯乙烯(PVDC)膜中癸二酸二丁酯和乙酰柠檬酸三丁酯,采用DB-5MS毛细管色谱柱分离,选择离子监测模式,以二氯甲烷为提取溶剂,经自动索式提取完成后用气相色谱-质谱仪上机测定,外标法定量,癸二酸二丁酯和乙酰柠檬酸三丁酯很好分离,峰型好,可以准确定量,在两种加标水平下,癸二酸二丁酯和乙酰柠檬酸三丁酯回收率为94. 17%、95. 8%和93. 3%、95. 9%,相对标准偏差为1. 04%、1. 22%和1. 47%、0. 77%,相关系数为0. 999以上,检出限为0. 2 mg/kg。对色谱柱、气相色谱参数、提取方式条件等进行对比优化,该方法操作简捷高效,灵敏度高,准确性高,可实现PVDC膜中癸二酸二丁酯和乙酰柠檬酸三丁酯分析测定。
Dibutyl sebacate and tributyl O-acetylcitrate in polyvinyl dichloride( PVDC) film were measured by gas chromatography-mass spectrometry, taking DB-5 MS as separation capillary column, and selecting ion monitoring model. The sample was extracted by dichloromethane as solvent. After automatic cable extraction,gas chromatography-mass spectrometer was used to test by external scalar method. Dibutyl sebacate and tributyl O-acetylcitrate were separated well and the peak shape was good. It could be quantified at two markup levels. The recovery of dibutyl sebacate and tributyl O-acetylcitrate were 94. 17%,95. 8%and93. 3%,95. 9%, and the relative standard deviation were 1. 04%, 1. 22% and 1. 47%, 0. 77%,respectively. The correlation coefficient was better than 0. 999,and the detection limit was 0. 2 mg/kg. The parameters of chromatographic column,gas chromatographic parameters and extraction method were compared and optimized. The method was simple,efficient,sensitive,accurate and accuracy. The determination of dibutyl sebacate and tributyl O-acetylcitrate could be achieved in PVDC film.
引文
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