亲水相互作用色谱-串联质谱法测定液体食品中14种甜味剂  

Determination of 14 sweeteners in liquid foods by hydrophilic interaction liquid chromatography-tandem mass spectrometry

作　　者：范广宇 冯峰[1] 张峰[1] 高飞[1] 李晓明[3] 梁振纲[4] FAN Guangyu;FENG Feng;ZHANG Feng;GAO Fei;LI Xiaoming;LIANG Zhengang(Institute of Food Safety,Chinese Academy of Inspection and Quarantine,Beijing 100176,China;Lianyungang Entry-Exit Inspection and Quarantine Bureau,Lianyungang 222042,China;Jinan Entry-Exit Inspection and Quarantine Bureau,Jinan 250014,China;Technology Center of Hainan Entry-Exit Inspection and Quarantine Bureau,Haikou 570311,China)

机构地区：[1]中国检验检疫科学研究院食品安全研究所,北京100176 [2]连云港出入境检验检疫局,江苏连云港222042 [3]济南出入境检验检疫局,山东济南250014 [4]海南出入境检验检疫局技术中心,海南海口570311

出　　处：《色谱》2018年第4期351-355,共5页Chinese Journal of Chromatography

基　　金：中央级公益性科研院所基本科研业务费专项资金项目(2016JK028);贵州茅台酒股份有限公司研发项目(2016010).

摘　　要：建立了亲水相互作用色谱-三重四极杆质谱(HILIC-MS/MS)同时测定液体食品中6种人工合成甜味剂和8种甜菊糖苷类天然甜味剂的分析方法。样品经Waters Xbridge Amide色谱柱(150 mm×5.0 mm,3.5μm)分离,以乙腈-10 mmol/L甲酸铵溶液(65∶35,v/v)为流动相,流速为0.4 mL/min,柱温为35℃,然后以电喷雾电离(ESI)源,在多反应监测(MRM)、负离子模式下进行三重四极杆质谱检测。14种甜味剂在各自的范围内线性关系良好,相关系数均大于0.995,检出限为0.03~0.7 mg/kg,定量限为0.1~2.2 mg/kg。在2、5和20 mg/kg添加水平下,14种甜味剂的平均回收率为80.8%~108.7%,相对标准偏差为1.5%~7.7%(n=6)。该方法样品前处理操作简单,准确度高,灵敏度高,可用于液体食品中14种甜味剂的同时测定。A method for the simultaneous determination of six artificial sweeteners and eight steviol glycosides in liquid food samples by hydrophilic interaction liquid chromatographytandem mass spectrometry(HILIC-MS/MS)was developed.The sweeteners in the samples were separated by a Waters Xbridge Amide column(150 mmx5.0 mm,3.5um)at 35℃,and eluted with acetonitrile-10 mmol/L ammonium formate(65:35,v/v)at a flow rate of 0.4 mL/min.Then,the analytes were detected using an electrospray ion source in negative mode(ESI-')under multiple reaction monitoring(MRM)mode.Good linear relationships were obtained,and the correlation coefficients(r 2)of the 14 sweeteners were greater than 0.995.The limits of detection(LODs,S/N=3)and the limits of quantification(LOQs,S/N=10)ranged from 0.03 to 0.7 mg/kg and 0.1 to 2.2 mg/kg,respectively.The average recoveries varied from 80.8%to 108.7%at spiked levels of 2,5 and 20 mg/kg,and the relative standard deviations(RSDs)ranged from 1.5%to 7.7%(n=6).The proposed method is simple,accurate and sensitive for the simultaneous determination of the 14 sweeteners in liquid food samples.

关 键 词：亲水相互作用色谱 三重四极杆质谱 人工合成甜味剂 甜菊糖苷 液体食品 

分 类 号：O658[理学—分析化学]