气相色谱-四极杆-飞行时间质谱仪分析油脂食品中多种邻苯二甲酸酯类化合物残留
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摘要
利用气相色谱-四极杆-飞行时间质谱(GC-QTOF MS)技术建立了油脂食品中23种邻苯二甲酸酯类快速检测方法。样品采用乙腈-甲基叔丁基醚(9∶1,v/v)提取,PSA分散剂净化,经GC-QTOF MS测定,采用外标法定量。在全扫描采集模式下,以特征离子峰的峰面积定量,以化合物的保留时间、精确质量数及谱库检索定准确性。23种化合物在线性范围内均呈现良好的线性关系,相关系数均大于0.99,23种化合物的定量限(S/N=10)为0.05~0.1mg/kg,在0.1~5.0mg/kg 3个添加水平下的平均回收率为79%~112%,相对标准偏差(RSD,n=6)均低于14%。该方法简便、快速、灵敏,可以应用于油脂类食品中23种邻苯二甲酸酯类的同时检测。
An efficient method was established for the simultaneous determination of 23 phthalate esters residues in grease food by gas chromatography coupled with quadrupole time of flight mass spectrometry(GC-QTOF MS). The samples were extracted with Acetonitrile-methyl tertiary butyl ether(9 ∶ 1,v/v) and cleaned-up with PSA adsorbents,then determined by GC-QTOF MS and quantified by external standard method. The confirmatory analysis for target compounds was performed with the retention time and qualitative fragments obtained by data-retrieval and fragmentations. The correlation coefficients of the 23 phthalate esters were more than 0. 99 in their linear ranges and the limits of quantification(LOQs) were 0. 05 ~ 0. 1mg/kg. The mean recoveries for the 23 phthalate esters in grease food were between 79% and 112% with the relative standard deviations(RSDs,n = 6) not more than14%. The method is rapid,sensitive,and suitable for the simultaneous determination of multi-classes of phthalate esters in grease food.
An efficient method was established for the simultaneous determination of 23 phthalate esters residues in grease food by gas chromatography coupled with quadrupole time of flight mass spectrometry(GC-QTOF MS). The samples were extracted with Acetonitrile-methyl tertiary butyl ether(9 ∶ 1,v/v) and cleaned-up with PSA adsorbents,then determined by GC-QTOF MS and quantified by external standard method. The confirmatory analysis for target compounds was performed with the retention time and qualitative fragments obtained by data-retrieval and fragmentations. The correlation coefficients of the 23 phthalate esters were more than 0. 99 in their linear ranges and the limits of quantification(LOQs) were 0. 05 ~ 0. 1mg/kg. The mean recoveries for the 23 phthalate esters in grease food were between 79% and 112% with the relative standard deviations(RSDs,n = 6) not more than14%. The method is rapid,sensitive,and suitable for the simultaneous determination of multi-classes of phthalate esters in grease food.
引文
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[10]李晓颍,张红医,常巧英,等.气相色谱-四极杆飞行时间质谱准确鉴定常见水果蔬菜中的农药残留[J].色谱,2014,32(3):268-277.
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[12]吴惠勤,朱志鑫,黄晓兰,等.不同类别食品中21种邻苯二甲酸酯的气相色谱-质谱测定及其分布情况研究[J].分析测试学报,2011,30(10):1079-1087.
[13]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,2012,30(1):27-31.
[2]陶然.食品中邻苯二甲酸酯类化合物残留分析方法的研究[D/OL].芜湖:安徽工程大学,2013:13-17[2017-01-03].http://cdmd.cnki.com.cn/Article/CDMD-10363-1014155712.htm.
[3]张莉,尚楚翔,孙成.气相色谱-三重四极杆质谱法同时测定生脉饮中17种邻苯二甲酸酯类化合物的残留量[J].色谱,2014,32(6):653-657.
[4]国家质量监督检验检疫总局.食品中邻苯二甲酸酯的测定:GB/T21911-2008[S/OL].北京:中国标准出版社,2008:1-7[2017-01-03].https://club.1688.com/article/24777934.html.
[5]国家质量监督检验检疫总局.出口食品中邻苯二甲酸酯的测定:SN/T3147-2012[S/OL].北京:中国标准出版社,2012:1-5(2013-05-23)[2017-01-03].http://www.bzxz8.com/Soft/SJBZSN/213612.html.
[6]王会锋,董小海,贾斌,等.固相萃取-气相色谱-串联质谱法测定大葱等蔬菜中23种邻苯二甲酸酯类化合物残留[J].色谱,2015,33(5):545-550.
[7]王玉健,黄惠玲,梁振纲,等.气相色谱-三重串联四极杆质谱(GC-MS/MS)测定烘焙食品中15种邻苯二甲酸酯[J].分析试验室,2013,32(10):58-62.
[8]罗铭,王璐,贺泽英,等.气相色谱-四极杆-飞行时间质谱仪(GC-QTOF)分析土壤中多环芳烃和农药残留[J].环境化学,2014,33(12):2216-2219.
[9]王雯雯,余翀天.气相色谱-四极杆-飞行时间质谱仪(GC-QTOF)分析大葱中多种农药残留[J].环境化学,2012,31(10):1660-1662.
[10]李晓颍,张红医,常巧英,等.气相色谱-四极杆飞行时间质谱准确鉴定常见水果蔬菜中的农药残留[J].色谱,2014,32(3):268-277.
[11]范若静.GC-QTOF MS定性方法的开发及其在复杂基质中的应用[D/OL].北京:中国科学院大学,2014:10-12[2017-01-03].http://d.wanfangdata.com.cn/Thesis/Y2674340.
[12]吴惠勤,朱志鑫,黄晓兰,等.不同类别食品中21种邻苯二甲酸酯的气相色谱-质谱测定及其分布情况研究[J].分析测试学报,2011,30(10):1079-1087.
[13]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,2012,30(1):27-31.