气相色谱串联三重四级杆质谱测定焦糖色中4-甲基咪唑
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摘要
建立气相色谱-串联质谱(GC-MS/MS)测定焦糖色中4-甲基咪唑的检测方法。样品经过碱化处理,硅藻土固定吸附,乙酸乙酯直接萃取,气相色谱-串联质谱法多反应监测模式(MRM)测定。4-甲基咪唑在0.5～20μg/m L内具有较好线性关系,线性相关系数为0.999 7,方法检出限为5 mg/kg,在3个加标水平(5, 100和200 mg/kg)下加标回收率为78.3%～91.7%,相对标准偏差(RSD, n=6)为2.11%～7.12%,该方法前处理简单快捷,方法灵敏度高,准确性好,能够满足对焦糖色中4-甲基咪唑分析检测的需要。
A capillary gas chromatography-tandem mass spectrometry(GC-MS/MS) for determination of 4-Methylimidazole in caramel color was established. The samples were alkalized, adsorbed by kieselguhr, and extracted with ethyl acetate. The detection was carried out by GC-MS/MS in the multiple-reaction monitoring(MRM) mode. Good linear relationship was obtained in the concentrations of 0.5-20 μg/mL, while the correlation coefficient was 0.999 7 and the detection limit of this method was 5 mg/kg. The recoveries at three spiked levels(5, 100 and 200 mg/kg) were in the range of 78.3%-91.7% with RSDs between 2.11%-7.12%(n=6). The method was simple, rapid, sensitive and accurate to meet the needs of the analysis,which could be used for the detection of 4-methylimidazole in caramel color.
A capillary gas chromatography-tandem mass spectrometry(GC-MS/MS) for determination of 4-Methylimidazole in caramel color was established. The samples were alkalized, adsorbed by kieselguhr, and extracted with ethyl acetate. The detection was carried out by GC-MS/MS in the multiple-reaction monitoring(MRM) mode. Good linear relationship was obtained in the concentrations of 0.5-20 μg/mL, while the correlation coefficient was 0.999 7 and the detection limit of this method was 5 mg/kg. The recoveries at three spiked levels(5, 100 and 200 mg/kg) were in the range of 78.3%-91.7% with RSDs between 2.11%-7.12%(n=6). The method was simple, rapid, sensitive and accurate to meet the needs of the analysis,which could be used for the detection of 4-methylimidazole in caramel color.
引文
[1]刘冠卉.焦糖色素在食品工业中的应用[J].江苏调味副食品,2004(1):17-19.
[2]孟颖,闫璐,胡洁,等.选择离子气质联用法同时测定食醋中2-甲基咪唑和4-甲基咪唑[J].食品工业科技,2014,35(6):59-62.
[3]YUAN J H,BURKA L T.Toxicokinetics of 4-methylimidazole in the male F344 rat[J].Xenobiotica,1995,25:885-894.
[4]NISHIE K,WAISS A C,KEYL A C.Toxicity of methylimidazoles[J].Toxicology and Applied Pharmacology1969,14:303-307.
[5]黄志勤,屈海云.分光光度法测定焦糖色中4-甲基咪唑[J].中国调味品,2005(6):52-54.
[6]陈洪兴,戴军,陈尚卫,等.高效液相色谱法测定焦糖色素中的4-甲基咪唑[J].中国调味品,2006(06):53-56.
[7]FERNANDES J O,FERREIRA M A.Gas chromatographicmass spectrometric determination of 4-(5)methylimidazole in ammonia caramel colour using ion-pair extraction and derivatization with isobutylchloroformate[J].Journal of Chromatography A,1997,786:299-308.
[8]CHAN P,MAHLER J,TRAVLOS G,et al.Induction of thyroid lesions in 14-week toxicity studies of 2 and 4-methylimidazole in Fischer 344/N rats and B6C3F1 mice[J].Arch Toxicol,2006,80(3):169-180.
[9]宋慧坚.用纸层析法测定食用焦糖中4-甲基咪唑含量[J].广东卫生防疫,1998(2):11-12.
[10]冯彩群.蕉糖中4-甲基咪唑检测方法的探讨[J].中国卫生检验杂志,2000(1):48-49.
[11]中华人民共和国国家卫生和计划生育委员会.食品安全国家标准食品添加剂焦糖色:GB 1886.64-2015[S].北京:中国标准出版社,2015.
[12]郭小莉,陈敏,胡锦荣,等.气相色谱法测定酱油中的4-甲基咪唑[J].食品工业科技,2004(7):125-127.
[13]李继民,王彦吉,赵彦军,等.毛细管气相色谱法测定N-甲基咪唑的含量[J].福建分析测试,2009,18(4):37-40.
[14]肖义夫,廖百森.高效液相色谱法测定焦糖色素中4-甲基咪唑[J].现代预防医学,2005(3):249-250.
[15]林晓珊,杭义萍,吴惠勤,等.气相色谱-串联质谱法测定焦糖色素中2-甲基咪唑和4-甲基咪唑[J].分析试验室,2011,30(11):85-88.
[16]吴翠华,郑学殷,李巧琪,等.QuEChERS结合高效液相色谱-串联质谱法测定酱油中的4-甲基咪唑[J].当代化工,2018,47(3):653-656.
[2]孟颖,闫璐,胡洁,等.选择离子气质联用法同时测定食醋中2-甲基咪唑和4-甲基咪唑[J].食品工业科技,2014,35(6):59-62.
[3]YUAN J H,BURKA L T.Toxicokinetics of 4-methylimidazole in the male F344 rat[J].Xenobiotica,1995,25:885-894.
[4]NISHIE K,WAISS A C,KEYL A C.Toxicity of methylimidazoles[J].Toxicology and Applied Pharmacology1969,14:303-307.
[5]黄志勤,屈海云.分光光度法测定焦糖色中4-甲基咪唑[J].中国调味品,2005(6):52-54.
[6]陈洪兴,戴军,陈尚卫,等.高效液相色谱法测定焦糖色素中的4-甲基咪唑[J].中国调味品,2006(06):53-56.
[7]FERNANDES J O,FERREIRA M A.Gas chromatographicmass spectrometric determination of 4-(5)methylimidazole in ammonia caramel colour using ion-pair extraction and derivatization with isobutylchloroformate[J].Journal of Chromatography A,1997,786:299-308.
[8]CHAN P,MAHLER J,TRAVLOS G,et al.Induction of thyroid lesions in 14-week toxicity studies of 2 and 4-methylimidazole in Fischer 344/N rats and B6C3F1 mice[J].Arch Toxicol,2006,80(3):169-180.
[9]宋慧坚.用纸层析法测定食用焦糖中4-甲基咪唑含量[J].广东卫生防疫,1998(2):11-12.
[10]冯彩群.蕉糖中4-甲基咪唑检测方法的探讨[J].中国卫生检验杂志,2000(1):48-49.
[11]中华人民共和国国家卫生和计划生育委员会.食品安全国家标准食品添加剂焦糖色:GB 1886.64-2015[S].北京:中国标准出版社,2015.
[12]郭小莉,陈敏,胡锦荣,等.气相色谱法测定酱油中的4-甲基咪唑[J].食品工业科技,2004(7):125-127.
[13]李继民,王彦吉,赵彦军,等.毛细管气相色谱法测定N-甲基咪唑的含量[J].福建分析测试,2009,18(4):37-40.
[14]肖义夫,廖百森.高效液相色谱法测定焦糖色素中4-甲基咪唑[J].现代预防医学,2005(3):249-250.
[15]林晓珊,杭义萍,吴惠勤,等.气相色谱-串联质谱法测定焦糖色素中2-甲基咪唑和4-甲基咪唑[J].分析试验室,2011,30(11):85-88.
[16]吴翠华,郑学殷,李巧琪,等.QuEChERS结合高效液相色谱-串联质谱法测定酱油中的4-甲基咪唑[J].当代化工,2018,47(3):653-656.