摘要
建立了固相萃取-高效液相色谱-串联质谱快速检测食品中安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜、纽甜、甘素及新橙皮甙二氢查尔酮等9种人工合成甜味剂的方法。样品中的甜味剂经三乙胺缓冲溶液(pH 4.5)提取,采用亲水亲脂平衡填料固相萃取柱净化,经Phenomenex Knietex~? F5色谱柱(100 mm×2.1 mm, 2.6μm)分离,以0.1%(v/v)甲酸-5 mmol/L甲酸铵溶液和甲醇为流动相,进行梯度洗脱,以电喷雾离子源正负离子切换多反应监测(MRM)模式进行质谱检测。采用内标法定量,进一步降低样品基质效应的影响。结果表明:本方法在去除样品基质干扰方面取得良好效果,9种甜味剂的检出限和定量限分别在2～30μg/L和6～100μg/L之间,在各自的线性范围内线性关系良好(相关系数r~2>0.999)。9种甜味剂空白样品在3个水平下的加标回收率在86.3%～106.3%之间,相对标准偏差(RSD)在1.2%～5.9%之间。本方法快捷、高效、准确可靠,可用于复杂食品基质中9种人工合成甜味剂的快速检测。
A simple and rapid method based on solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry for the simultaneous determination of nine artificial sweeteners(acesulfame-K, saccharin sodium, cyclamate, sucralose, aspartame, alitame, neotame, dulcin, neohesperidin dihydrochalcone) in various foods was developed. The sweeteners in food samples were extracted with triethylamine buffer solution(pH 4.5) and cleaned using an SPE column equipped with hydrophilic and lipophilic packing material. The analytes were separated on a Phenomenex Knietex~? F5 column(100 mm×2.1 mm, 2.6 μm) using 0.1%(v/v) formic acid-5 mmol/L ammonium formate/methanol as a mobile phase for gradient elution, and then determined by tandem mass spectrometry in positive and negative ESI modes under multiple reaction monitoring(MRM). The internal standard method was used to further suppress the matrix effect. The method proved to be very effective in the removal of matrix interferences. Calibration curves were linear within a studied range of concentrations(r~2>0.999) for the nine artificial sweeteners. The limits of detection(LODs) and limits of quantification(LOQs) were within 2-30 μg/kg and 6-100 μg/kg, respectively. The recoveries for the nine investigated sweeteners were within 86.3%-106.3% at three spiked levels, with relative standard deviations(RSDs) between 1.2% and 5.9%. The developed method is rapid, efficient, accurate, and reliable; it can also be applied for the rapid determination of other artificial sweeteners in a complex food matrix.
引文
[1] Kokotou M G,Asimakopoulos A G,Thomaidis N S.Anal Methods,2012,4(10):3057
[2] Buerge I J,Buser H R,Kahle M,et al.Environ Sci Technol,2009,43(12):4381
[3] Zygler A,Wasik A,Namiesnik J.TrAC-Trends Anal Chem,2009,28(9):1082
[4] Zhao Z,Wan P,Liu C X,et al.China Brewing,2014,33(1):147 赵贞,万鹏,刘春霞,等.中国酿造,2014,33(1):147
[5] Zhao Z L,Xie F,Jia K J,et al.Food Technology,2013,38(2):301 赵志磊,谢飞,贾克军,等.食品科技,2013,38(2):301
[6] Yang X Q,Li Y Q,Zou X L,et al.Modern Preventive Medicine,2017,44(22):55 杨小琪,黎源倩,邹晓莉,等.现代预防医学,2017,44(22):55
[7] Xiao X C.Physical Testing and Chemical Analysis Part B:Chemical Analysis,1997(3):118 肖学成.理化检验(化学分册),1997(3):118
[8] Yang R J,Sun J,Li H Z,et al.Liquor-Making Science & Technology,2016(9):122 杨仁君,孙洁,李好转,等.酿酒科技,2016(9):122
[9] Herrmannova M,Kriva N L,Bartos M,et al.J Sep Sci,2015,29(8):1132
[10] Jiang Y X,Wei R X,Yang G Z,et al.Journal of Instrumental Analysis,2009,28(7):838 蒋奕修,魏瑞霞,杨桂珍,等.分析测试学报,2009,28(7):838
[11] Chen S,Guo P,Wan J C,et al.Spectroscopy and Spectral Analysis,2017,37(5):1412 陈思,郭平,万建春,等.光谱学与光谱分析,2017,37(5):1412
[12] Agata Z,Andrzej W,Agata K W,et al.Anal Bioanal Chem,2011,400(7):2159
[13] Yang D J,Bo C.J Agric Food Chem,2009,57(8):3022
[14] Ji C,Feng F,Chen Z H,et al.Chinese Journal of Chromatography,2010,28(8):749 嵇超,冯峰,陈正行,等.色谱,2010,28(8):749
[15] Shao M Y.Chinese Journal of Analysis Laboratory,2017,36(1):96 邵明媛.分析试验室,2017,36(1):96
[16] Fan G Y,Feng F,Zhang F,et al.Chinese Journal of Chromatography,2018,36(4):351 范广宇,冯峰,张峰,等.色谱,2018,36(4):351
[17] Feng F,Li W M,Sun Y,et al.Chinese Journal of Chromatography,2019,37(1):87 冯峰,李伟明,孙燕,等.色谱,2019,37(1):87
[18] Ke R H,Wang L J,An H M,et al.Food and Fermentation Industries,2016,42(4):174 柯润辉,王丽娟,安红梅,等.食品与发酵工业,2016,42(4):174
[19] Niu Z R,Wang X J,Yu Y T,et al.Food Science,2016,37(2):178 牛之瑞,王秀君,于毅涛,等.食品科学,2016,37(2):178
[20] Zhou Y,Dong X Y,Yu Y,et al.Food Research and Development,2018,39(10):143 周玉,董孝元,余义,等.食品研究与开发,2018,39(10):143
[21] Guan Y Y,Qiu Z C,Song Y,et al.China Dairy Industry,2016,44(12):45 官咏仪,邱志超,宋阳,等.中国乳品工业,2016,44(12):45
[22] Wang H,Huang X B,Liu J,et al.Chinese Journal of Chromatography,2018,36(7):700 汪辉,黄小贝,刘江,等.色谱,2018,36(7):700
[23] Matuszewski B K,Constanzer M L,Chavez-Eng C M.Anal Chem,2003,75(13):3019
