气相色谱-串联质谱法测定白酒中10种增塑剂
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摘要
建立了气相色谱-串联质谱同时测定白酒中10种增塑剂的检测方法。样品经正己烷提取后,上清液选用DB-5ms非极性毛细管色谱柱对待测物进行分离,经EI离子源电离后以多反应监测(MRM)模式采集数据并做定性筛查和定量分析。10种增塑剂在相应的浓度范围内线性关系良好,相关系数均大于0.99,对白酒进行3个不同浓度的加标试验,平均回收率79.8%-106.7%,相对标准偏差RSD在1.27%-5.13%,检出限(LOD,S/N=3)为0.002-0.045 mg/kg。该方法成本低廉、灵敏度可靠,适用于白酒中10种增塑剂进行定性和定量测定。
A method has been developed and validated for the determination of 10 plasticizers in wineusing gas chromatographytandem mass spectrometry. The samples were extracted by hexane. The extracts were separatedby DB-5 MSnon-polar capillary column. The qualitative and quantitative analyses of the 10 plasticizers were ionized by EI using multiple reaction monitoring(MRM). The wine were spiked experiments at three levels.The correlation coefficients of linear calibration curves were over 0.99 in the corresponding concentration ranges.The average recoveries of the 10 plasticizers ranged from 79.8% to 106.7%. And the relative standard deviations(LODs S/N=3) were 0.002-0.045 mg/kg. The method is low cost,sensitive,reliable and suitable for the determination of 10 plasticizers in wine.
A method has been developed and validated for the determination of 10 plasticizers in wineusing gas chromatographytandem mass spectrometry. The samples were extracted by hexane. The extracts were separatedby DB-5 MSnon-polar capillary column. The qualitative and quantitative analyses of the 10 plasticizers were ionized by EI using multiple reaction monitoring(MRM). The wine were spiked experiments at three levels.The correlation coefficients of linear calibration curves were over 0.99 in the corresponding concentration ranges.The average recoveries of the 10 plasticizers ranged from 79.8% to 106.7%. And the relative standard deviations(LODs S/N=3) were 0.002-0.045 mg/kg. The method is low cost,sensitive,reliable and suitable for the determination of 10 plasticizers in wine.
引文
[1]石万聪,司俊杰,刘文国.ISBN978-7-122-01375-0,增塑剂实用手册[M].北京:化学工业出版社,2009(1)7.
[2]肖乃玉,陆杏春,郭清兵,等.塑料食品包装中邻苯二甲酸酯类增塑剂迁移研究进展[J].包装工程,2010,31(11):123-127.
[3]叶雅真,朱宝平,洪华荣,等,2012年厦门市售婴幼儿配方奶粉及辅助食品中邻苯二甲酸酯类物质监测结果分析[J].中国卫生检验杂志,2013,23(1):218-219.
[4]GB 9685-2008食品容器、包装材料用添加剂使用卫生标准[S].
[5]赵俊虹.气质联用法检测塑料包装西式火腿中邻苯二甲酸酯类增塑剂[J].粮油加工,2010(5):131-133.
[6]李一尘,徐静,董伟峰,等.气相色谱及气相色谱-质谱法检测食品中增塑剂[J].检验检疫学刊,2012(22):40-43.
[7]柴丽月,辛志宏,蔡晶,等.食品中邻苯二甲酸酯类增塑剂含量的检测[J].分析检测,2008(7):362-365.
[8]杨琼,张明时,陈文生,等.气相色谱法测定食用油脂中6种邻苯二甲酸酯类化合物[J].中国粮油学刊,2008(5):171-174.
[9]李艳松,陈铁英,黄宝临,等.食品中16种邻苯二甲酸酯类化合物的气相色谱测定方法[J].食品与机械,2012(1):105-107.
[10]王连珠,王瑞龙,刘溢娜,等.分散固相萃取-气相色谱-质谱法检测罐头食品中6种邻苯二甲酸酯[J].理化检验,2008(6):502-506.
[2]肖乃玉,陆杏春,郭清兵,等.塑料食品包装中邻苯二甲酸酯类增塑剂迁移研究进展[J].包装工程,2010,31(11):123-127.
[3]叶雅真,朱宝平,洪华荣,等,2012年厦门市售婴幼儿配方奶粉及辅助食品中邻苯二甲酸酯类物质监测结果分析[J].中国卫生检验杂志,2013,23(1):218-219.
[4]GB 9685-2008食品容器、包装材料用添加剂使用卫生标准[S].
[5]赵俊虹.气质联用法检测塑料包装西式火腿中邻苯二甲酸酯类增塑剂[J].粮油加工,2010(5):131-133.
[6]李一尘,徐静,董伟峰,等.气相色谱及气相色谱-质谱法检测食品中增塑剂[J].检验检疫学刊,2012(22):40-43.
[7]柴丽月,辛志宏,蔡晶,等.食品中邻苯二甲酸酯类增塑剂含量的检测[J].分析检测,2008(7):362-365.
[8]杨琼,张明时,陈文生,等.气相色谱法测定食用油脂中6种邻苯二甲酸酯类化合物[J].中国粮油学刊,2008(5):171-174.
[9]李艳松,陈铁英,黄宝临,等.食品中16种邻苯二甲酸酯类化合物的气相色谱测定方法[J].食品与机械,2012(1):105-107.
[10]王连珠,王瑞龙,刘溢娜,等.分散固相萃取-气相色谱-质谱法检测罐头食品中6种邻苯二甲酸酯[J].理化检验,2008(6):502-506.