气相色谱-质谱法测定聚偏二氯乙烯膜中癸二酸二丁酯和乙酰柠檬酸三丁酯
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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.
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
[1]张娟.PVDC薄膜的阻隔性能研究[J].科技与创新,2015(15):17-118.
[2]管东玲,刘俊伟,杨国宇.新型高阻隔PVDC材料性能及应用[J].塑料制造,2007(11):78-84.
[3]杨孜晨,吴若梅,萧可琪,等.聚偏二氯乙烯薄膜在食品包装中的应用及趋势[J].包装世界,2017(1):26-27.
[4]许戈文,李布青.合成香料产品技术手册[M].北京:中国商业出版社,1996:245.
[5]俞善信.国内催化合成癸二酸二丁酯研究进展[J].塑料助剂,2009(6):11-14.
[6]邢光全,宋方俊,周志国.一种新型无毒增塑剂的应用及生产[J].聚氯乙烯,2006(12):23-25.
[7]中华人民共和国卫生部.食品安全国家标准食品接触材料及制品用添加剂使用标准:GB 9685-2016[S].北京:中国标准出版社,2016.
[8]周相娟,赵玉琪,李伟,等.气相色谱/质谱法测定塑料食品包装中柠檬酸酯[J].食品与机械2010,26(5):65-67.
[9]刘彦坤,王小萍,罗远芳,等.聚氯乙烯环保型增塑剂的研究进展[J].化工进展,2008,27(1):74-77.
[10]姚李,吴缨.气相色谱-质谱法对柠檬酸三丁酯的检测研究[J].合肥学院学报(自然科学版),2008,18(1):13-15.
[11]王进,李宣.超声萃取气相色谱-质谱联用法测定塑料中邻苯二甲酸酯类增塑剂及其不确定度评估[J].科学技术与工程,2009,9(14):285-288.
[12]张伟亚,王成云,刘丽,等.微波萃取气相色谱-质谱法测定塑料中的增塑剂[J].塑料科技,2009,37(5):77-81.
[2]管东玲,刘俊伟,杨国宇.新型高阻隔PVDC材料性能及应用[J].塑料制造,2007(11):78-84.
[3]杨孜晨,吴若梅,萧可琪,等.聚偏二氯乙烯薄膜在食品包装中的应用及趋势[J].包装世界,2017(1):26-27.
[4]许戈文,李布青.合成香料产品技术手册[M].北京:中国商业出版社,1996:245.
[5]俞善信.国内催化合成癸二酸二丁酯研究进展[J].塑料助剂,2009(6):11-14.
[6]邢光全,宋方俊,周志国.一种新型无毒增塑剂的应用及生产[J].聚氯乙烯,2006(12):23-25.
[7]中华人民共和国卫生部.食品安全国家标准食品接触材料及制品用添加剂使用标准:GB 9685-2016[S].北京:中国标准出版社,2016.
[8]周相娟,赵玉琪,李伟,等.气相色谱/质谱法测定塑料食品包装中柠檬酸酯[J].食品与机械2010,26(5):65-67.
[9]刘彦坤,王小萍,罗远芳,等.聚氯乙烯环保型增塑剂的研究进展[J].化工进展,2008,27(1):74-77.
[10]姚李,吴缨.气相色谱-质谱法对柠檬酸三丁酯的检测研究[J].合肥学院学报(自然科学版),2008,18(1):13-15.
[11]王进,李宣.超声萃取气相色谱-质谱联用法测定塑料中邻苯二甲酸酯类增塑剂及其不确定度评估[J].科学技术与工程,2009,9(14):285-288.
[12]张伟亚,王成云,刘丽,等.微波萃取气相色谱-质谱法测定塑料中的增塑剂[J].塑料科技,2009,37(5):77-81.