LC-MS/MS法同时检测糕点类食品中9种Amadori化合物
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摘要
建立测定糕点食品中9种Amadori化合物的液相色谱-串联质谱(LC-MS/MS)方法。样品经甲醇萃取、正己烷除脂,经QuEChERS(50 mg PSA和100 mg C18混合物)净化后,进行LC-MS/MS测定分析。流动相为甲醇与0.5%甲酸水溶液,用Waters Acquity BEH C18(100 mm×2.1 mm,1.7μm)分离。结果表明:该方法检出限在0.13～0.70μg/g,日内精密度RSD(n=6)在2.44%～5.79%,日间精密度RSD(n=3)在3.02%～5.97%,稳定性好,回收率在80.3%～112.4%,准确性高。该方法准确可靠、灵敏度高,非常适合复杂基质糕点类食品中9种Amadori化合物的分析。
A rapid method for simultaneously determining 9 Amadori compounds in pastry food by high performance liquid chromatography-triple quaternary mass spectrometry was developed. The pastry food was extracted with methanol, n-hexane degreased, and purified by QuEChERS(50 mg PSA and 100 mg C18 mixture), then analyzed by LC-MS/MS. The samples were separated on an Waters Acquity BEH C18 column with the gradient elution mobile phase of methanol and 0.5%(v/v) formic acid aqueous solution. Results showed that: the limit of detection was between 0.13 μg/kg and 0.70 μg/kg, the intra-day and the inter-day relative standard deviations(RSDs) were 2.44%～5.79%(n=6) and 3.02%～5.97%(n=3), the standard recoveries of the spiked samples ranged from 80.3% to 112.4%. The method was accurate, reliable and sensitive, and was very suitable for the analysis of the 9 Amadori compounds in pastry food.
A rapid method for simultaneously determining 9 Amadori compounds in pastry food by high performance liquid chromatography-triple quaternary mass spectrometry was developed. The pastry food was extracted with methanol, n-hexane degreased, and purified by QuEChERS(50 mg PSA and 100 mg C18 mixture), then analyzed by LC-MS/MS. The samples were separated on an Waters Acquity BEH C18 column with the gradient elution mobile phase of methanol and 0.5%(v/v) formic acid aqueous solution. Results showed that: the limit of detection was between 0.13 μg/kg and 0.70 μg/kg, the intra-day and the inter-day relative standard deviations(RSDs) were 2.44%～5.79%(n=6) and 3.02%～5.97%(n=3), the standard recoveries of the spiked samples ranged from 80.3% to 112.4%. The method was accurate, reliable and sensitive, and was very suitable for the analysis of the 9 Amadori compounds in pastry food.
引文
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[14]翟玉俊,黄伟,陈华,等.LC-MS法定性定量测定烟草中的1-氨基-1-脱氧-2-酮糖[J].烟草科技,2011,285(4):58-61.
[15]张婕,葛永辉,杨慧,等.LC-MS/MS法同时测定烟草中的16种游离氨基酸和6种Amadori化合物[J].烟草科技,2017,50(11):58-65.
[16]贾春晓,修龙飞,牟定荣,等.液相色谱-串联质谱法同时测定烟草中6种Amadori化合物[J].质谱学报,2015,36(1):45-51.
[17]YUAN Heng,SUN Lin-juan,CHEN Min,et al.The comparison of the contents of sugar,Amadori,and Heyns compounds in fresh and black garlic[J].Journal of Food Science,2016,81(7):C1662-C1668.
[18]糕点通则:GB/T 20977-2007[S].北京:中国标准出版社,2007.
[2]FUJIMAKI M,NAMIKI M,KATO H.Amino-Carbonyl reactions in food and biological systems[M].Kodansha Ltd,1986.
[3]JAEGER H,JANOSITZ A,KNAORR D.The Maillard reaction and its control during food processing.The potential of emerging technologies[J].Pathologie Biologie,2010,58(3):207-213.
[4]LAURA J C,MAR V,PEDRO J M,et al.Effect of the dryheating conditions on the glycosylation ofβ-lactoglobulin with dextran through the Maillard reaction[J].Food Hydro colloids,2005,19(5):831-837.
[5]尤新.氨基酸和糖类的美拉德反应-开发新型风味剂和食品抗氧剂的新途径[J].食品工业科技,2004,25(7):138-139.
[6]龚平,阚建全.美拉德反应产物性质的研究进展[J].食品与发酵工业,2009,35(4):141-146.
[7]曾茂茂,李伶俐,何志勇,等.甘氨酸对美拉德反应体系及产生肉香风味物质的影响[J].食品科学,2012,33(7):32-36.
[8]LEE K G,SHIBAMOTO T.Toxicology and antioxidant activities of non-enzymatic browning reaction products:review[J].Food Reviews International,2002,18(2-3):151-175.
[9]HAYASE F,TAKAHASHI Y,TOMINAGA S,et al.Identification of Blue Pigment Formed in a D-XyloseGlycine Reaction System[J].Bioscience Biotechnology&Biochemistry,1999,63(8):1512-1514.
[10]WANG J,LU Y M,LIU B Z,et a1.Electrospray positive ionization tandem mass spectrometry of Amadori compounds[J].Journal of Mass Spectrometry,2008,43(2):262-264.
[11]SUN J G,HE J W,WU F G,et a1.Comparative Analysis on Chemical Components and Sensory Quality of Aging Flue-Cured Tobacco from Four Main Tobacco Areas of China[J].Journal of Integrative Agriculture,2011,10(8):1222-1231.
[12]BAPTISTA J A B,CARVALHO R C B.Indirect determination of Amadori compounds in milk-based products by HPLC/ELSD/UV as an index of protein deterioration[J].Food Research International,2004,37(8):739-747.
[13]GE S J,LEE T C.Effective HPLC method for the determination of aromatic amadori compounds[J].Journal of Agricultural and Food Chemistry,1996,44(4):1053-1057.
[14]翟玉俊,黄伟,陈华,等.LC-MS法定性定量测定烟草中的1-氨基-1-脱氧-2-酮糖[J].烟草科技,2011,285(4):58-61.
[15]张婕,葛永辉,杨慧,等.LC-MS/MS法同时测定烟草中的16种游离氨基酸和6种Amadori化合物[J].烟草科技,2017,50(11):58-65.
[16]贾春晓,修龙飞,牟定荣,等.液相色谱-串联质谱法同时测定烟草中6种Amadori化合物[J].质谱学报,2015,36(1):45-51.
[17]YUAN Heng,SUN Lin-juan,CHEN Min,et al.The comparison of the contents of sugar,Amadori,and Heyns compounds in fresh and black garlic[J].Journal of Food Science,2016,81(7):C1662-C1668.
[18]糕点通则:GB/T 20977-2007[S].北京:中国标准出版社,2007.