固相萃取-高效液相色谱-串联质谱法测定酱油中4-甲基咪唑Determination of 4-methylimidazole in Soy Sauce Using Solid-phase Extraction and High Performance Liquid Chromatography-Tandem Mass Spectrometry
李锦清,綦艳,郦明浩,邱启东
摘要(Abstract):
建立固相萃取-高效液相色谱-串联质谱/质谱法(SPE-HPLC-MS/MS)测定酱油中4-甲基咪唑的分析方法。试样经水稀释提取,LC-SCX固相萃取柱净化后,以乙腈和5mmol/L乙酸铵溶液(含0.1%甲酸,V/V)作为流动相,C18色谱柱分离,采用电喷雾离子源,正离子扫描多反应监测(MRM)模式进行检测。4-甲基咪唑在5~500μg/L浓度范围内呈良好线性关系,相关系数(r2)大于0.99,加标回收率为83.6%~95.1%,相对标准偏差为7.3%~8.2%,方法检出限为5μg/kg,定量限为10μg/kg。方法简单快速、准确灵敏,适用于酱油中4-甲基咪唑的测定。
关键词(KeyWords): 4-甲基咪唑;高效液相色谱-串联质谱法;固相萃取;酱油
基金项目(Foundation):
作者(Author): 李锦清,綦艳,郦明浩,邱启东
参考文献(References):
- [1]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.
- [2]Grosse Y,Baan R,Secretan-Lauby B,et al.Carcinogenicity of chemicals in industrial and consumer products,food contaminants and flavorings,and water chlorination byproducts[J].Lancet Onc,2011,12(4):328-329.
- [3]彭向前,冯玮,石海英,等.气相色谱法同时检测焦糖色素中的2-甲基咪唑和4-甲基咪唑[J].中国调味品,2012,37(8):83-85.
- [4]熊珺,陈美玲,赖毅东.固相萃取-选择离子气质联用法测定液态调味料中的4-甲基咪唑[J].现代食品科技,2012,28(5):567-569,578.
- [5]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.
- [6]Moretton C,Cretier G,Nigay H,et al.Quantification of 4-methylimidazole in class III and IV caramel colors:validation of a new method based on heart-cutting twodimensional liquid chromatography(LC-LC)[J].J Agric Food Chem.,2011,59(8):3544-3550.
- [7]张晓燕,芦春梅,郭娜,等.高效液相色谱法测定饮料中的4-甲基咪唑[J].中国酿造,2013,32(5):148-149.
- [8]Yamaguchi H,Masuda T.Determination of 4(5)-methylimidazole in soy sauce and other foods by LC-MS/MS after solid-phase extraction[J].J Agric Food Chem.,2011,59(18):9770-9775.
- [9]Wang J Y,Schnute W C.Simultaneous quantitation of 2-acetyl-4-tetrahydroxybutylimidazole,2-and 4-methylimidazoles,and 5-hydroxymethylfurfural in beverages by ultrahigh-performance liquid chromatography-tandem mass spectrometry[J].J Agric Food Chem.,2012,60(4):917-921.
- [10]蔡玮红,冼燕萍,罗海英,等.UPLC-MS/MS法同时测定焙烤食品中的丙烯酰胺、4-甲基咪唑与5-羟甲基糠醛[J].现代食品科技,2014,30(2):249-254.
- [11]Schlee C,Markova M,Schrank J,et al.Determination of2-methylimidazole,4-methylimidazole and 2-acetyl-4-(1,2,3,4-tetrahydroxybutyl)imidazole in caramel colours and cola using LC/MS/MS[J].J Chromatogr B,2013,927:223-226.