分散固相萃取-气相色谱-串联质谱法测定油脂食品中33种增塑剂
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摘要
建立了分散固相萃取-气相色谱-串联质谱同时测定含油食品中33种增塑剂的检测方法。样品经乙腈提取后,上清液经分散固相萃取(dSPE)净化后浓缩。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。33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4类典型代表的油脂食品进行加标试验,平均回收率85-106%,相对标准偏差RSD在1.13-6.28%,检出限(LOD,S/N=3)为0.010-0.316mg/kg。该方法成本低廉、灵敏度可靠,适用于同时对油脂食品中33种增塑剂进行定性和定量测定。
A method has been developed and validated for the determination of 33 Plasticizers in oily foodusing dispersive solid-phase extraction(dSPE) coupled with gas chromatographytandem mass spectrometry. The samples were extracted by acetonitrile. The extracts were purified using mixed adsorbent by dSPE and then concentrated.After the separation on DB-5 MSnon-polar capillary column. The qualitative and quantitative analyses of the 33 Plasticizers were ionized by EI using multiple reaction monitoring(MRM). The four kinds of typical oily foods 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 33 Plasticizers ranged from 85% to 106%, And the relative standard deviations(RSDs) were 1.13-6.28%. The limits of detection(LODs S/N=3) were 0.010-0.316 mg/kg.The method is low cost, sensitive, reliable and suitable for the determination of 33 Plasticizers in oily food.
A method has been developed and validated for the determination of 33 Plasticizers in oily foodusing dispersive solid-phase extraction(dSPE) coupled with gas chromatographytandem mass spectrometry. The samples were extracted by acetonitrile. The extracts were purified using mixed adsorbent by dSPE and then concentrated.After the separation on DB-5 MSnon-polar capillary column. The qualitative and quantitative analyses of the 33 Plasticizers were ionized by EI using multiple reaction monitoring(MRM). The four kinds of typical oily foods 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 33 Plasticizers ranged from 85% to 106%, And the relative standard deviations(RSDs) were 1.13-6.28%. The limits of detection(LODs S/N=3) were 0.010-0.316 mg/kg.The method is low cost, sensitive, reliable and suitable for the determination of 33 Plasticizers in oily food.
引文
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[14]郭海霞,肖桂英,张禧庆,等.uEChERS-超高效液相色谱-串联质谱法同时检测猪肉中121种兽药[J].色谱,2015,33(12):1242-1250.
[15]李娜,张玉婷,刘磊,等.QuEChERS-超高效液相色谱-串联质谱法测定动物源食品中4类29种禁限用兽药残留[J].色谱,2014(12):1313-1319.
[16]木合他拜尔,严华,徐珊,等.QuECh ERS-超高效液相色谱-高分辨串联质谱技术检测鸡肉中6种抗球虫药物[J].色谱,2015(11):1199-1204.
[17]许旭,肖远灿,耿丹丹,等.在线柱后衍生-高效液相色谱-荧光检测法同时测定牛肉中16种磺胺类药物残留[J].色谱,2016(4):422-428.
[18]王伟,石志红,康健,等.改进的QuECh ERS结合LC-MS/MS同时测定蜂蜜中60种兽药残留[J].分析试验室,2013(4):82-88.
[19]朱万燕,张欣,杨娟,等.超高效液相色谱-四极杆-飞行时间质谱法同时测定猪肉中多类兽药残留[J].色谱,2015(9):1002-1008.
[20]宫小明,董静,孙军,等.动物源性食品中阿维菌素类药物残留的QuEChERS-液质联用法测定[J].分析测试学报,2010(9):933-937.
[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.
[11]杨悠悠,谢云峰,田菲菲,等.常见食品中邻苯二甲酸酯类增塑剂含量及食品包装材料中邻苯二甲酸酯类增塑剂迁移量的测定[J].色谱,2013(7):674-678.
[12]郑向华,林立毅,方恩华,等.固相萃取-气相色谱-质谱法测定食品中23种邻苯二甲酸酯[J].色谱,2012(1):27-32.
[13]卢春山,李玮,屠海云,等.气相色谱-质谱联用测定食品中的邻苯二甲酸酯[J].分析测试学刊,2010(10):1036-1040.
[14]郭海霞,肖桂英,张禧庆,等.uEChERS-超高效液相色谱-串联质谱法同时检测猪肉中121种兽药[J].色谱,2015,33(12):1242-1250.
[15]李娜,张玉婷,刘磊,等.QuEChERS-超高效液相色谱-串联质谱法测定动物源食品中4类29种禁限用兽药残留[J].色谱,2014(12):1313-1319.
[16]木合他拜尔,严华,徐珊,等.QuECh ERS-超高效液相色谱-高分辨串联质谱技术检测鸡肉中6种抗球虫药物[J].色谱,2015(11):1199-1204.
[17]许旭,肖远灿,耿丹丹,等.在线柱后衍生-高效液相色谱-荧光检测法同时测定牛肉中16种磺胺类药物残留[J].色谱,2016(4):422-428.
[18]王伟,石志红,康健,等.改进的QuECh ERS结合LC-MS/MS同时测定蜂蜜中60种兽药残留[J].分析试验室,2013(4):82-88.
[19]朱万燕,张欣,杨娟,等.超高效液相色谱-四极杆-飞行时间质谱法同时测定猪肉中多类兽药残留[J].色谱,2015(9):1002-1008.
[20]宫小明,董静,孙军,等.动物源性食品中阿维菌素类药物残留的QuEChERS-液质联用法测定[J].分析测试学报,2010(9):933-937.