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当前位置: 首页 > 文章 > 高效液相色谱-串联质谱法测定油条中羧甲基赖氨酸 食品工业科技 2014,35 (11) 298-301+323
Position: Home > Articles > High performance liquid chromatography-tandem mass spectrometry method for the determination of Nε-( carboxymethyl) lysine in fried bread sticks Science and Technology of Food Industry 2014,35 (11) 298-301+323

高效液相色谱-串联质谱法测定油条中羧甲基赖氨酸

作  者：
孙晓华;赖克强;黄轶群;王婧;吴轶;肖竹青
单  位：
上海海洋大学食品学院;上海市食品研究所
关键词：
羧甲基赖氨酸;亲水作用色谱;高效液相色谱-串联质谱;油条
摘  要：
建立了利用高效液相色谱-串联质谱法(HILIC-HPLC-MS/MS)测定油条中羧甲基赖氨酸(CML)含量的检测方法。样品经硼氢化钠还原、盐酸水解,过混合型阳离子交换小柱萃取净化,样品溶液在HILIC色谱柱中以甲醇-水(均含2mmol/L乙酸铵和0.1%甲酸)为流动相进行梯度洗脱,CML被保留并与样品基质分离。选用电喷雾正离子(ESI+)模式电离,多反应监测模式(MRM)进行串联质谱分析。以内标法定量,D4-CML为内标物,分析时间为12min。本方法添加回收率范围89.5%~99.1%,相对标准偏差范围2.1%~2.6%,仪器检出限为1μg/L,定量限为3μg/L。应用该方法测得15种不同来源的油条中CML含量为69.3±8.2~182.2±3.1mg/(kg蛋白质),5.3±0.5~15.4±0.3mg/(kg样品)。本方法操作简便、快速、灵敏度高、精密度好,为进一步研究食品中CML的产生机理提供了有效的检测方法。
译  名：
High performance liquid chromatography-tandem mass spectrometry method for the determination of Nε-( carboxymethyl) lysine in fried bread sticks
作  者：
SUN Xiao-hua;LAI Ke-qiang;HUANG Yi-qun;WANG Jing;WU Yi;XIAO Zhu-qing;College of Food Science and Technology,Shanghai Ocean University;Shanghai Food Research Institute;
关键词：
Nε-(carboxymethyl) lysine(CML);;hydrophilic interaction chromatography(HILIC);;high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS);;fried bread sticks
摘  要：
A method for the determination of Nε-( carboxymethyl) lysine( CML) content in fried bread sticks was developed using high performance liquid chromatography- tandem mass spectrometry( HPLC- MS/MS).Food samples were reduced by sodium borohydride,then hydrolyzed by hydrochloric acid and finally cleaned up by mixed cation exchange( MCX) solid phase extraction cartridge.CML was remained on an Atlantis HILIC column.Methanol-water( all containing 2mmoI /L ammonium acetate and 0.1% formic acid) were used as mobile phases.Tandem MS analysis was performed in multiple reactions monitoring( MRM) mode using the electrospray positive ionization( ESI +) method.D4- CML was used as internal standard substance,and the analysis time was12min.The average recoveries of CML for this method ranged from 89.5% to 99.1%,with the relative standard deviations( RSD) were between 2.1% and 2.6%.The instrument detection limit was 1μg /L,and quantitation limit was3μg /L.Using this method,CML contents determined in 15 different sources fried bread sticks were 69.3 ± 8.2~182.2± 3.1mg /( kg protein),and 5.3 ± 0.5~15.4 ± 0.3mg /( kg sample).This method is simple,rapid,highly sensitive and accurate,and it is an effective method for further research on the generation mechanism of CML.

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