Lim Ho Soo, Choi EunA, Hwang Ju Young, Lee Gunyoung, Yun Sang Soon, Kim MeeKyung
a Food Additives and Packaging Division , National Institute of Food and Drug Safety Evaluation , Cheongju , Republic of Korea.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2018 Sep;35(9):1674-1688. doi: 10.1080/19440049.2018.1486043. Epub 2018 Aug 6.
An improved and highly sensitive method was developed and validated for the determination of 12 (7 permitted and 5 non-permitted in Korea) non-nutritive sweeteners in various foods using liquid chromatography-electrospray ionisation-tandem mass spectrometry. The chromatographic separation was performed on an Xbridge BEH C18 column (3 mm × 100 mm, 2.5 μm) with gradient elution using 10 mM ammonium acetate in water and 10 mM ammonium acetate in methanol. Sample preparation consisted of simple dilution, homogenisation, centrifugation and purification with a C18 cartridge prior to analysis. The relative matrix effect (%ME) was within ±20% for all sweeteners. The method also showed good linearity (R > 0.99). The limit of detection and limit of quantification values in sample were in the range of 0.02-2.66 and 0.06-8.05 mg kg, respectively. The recoveries at three concentration levels ranged between 80% and 119%, with relative standard deviation values below 10%. In addition, the expanded uncertainties determined for 12 sweeteners in 5 different food matrices were confirmed to be <14%. Finally, the method was successfully applied to the analysis of sweeteners in 681 food samples purchased in Korea, Australia and Turkey. These results demonstrate that the method is suitable for the simultaneous determination of multiple-sweeteners in a variety of foods.
开发并验证了一种改进的高灵敏度方法,用于使用液相色谱 - 电喷雾电离 - 串联质谱法测定各种食品中的12种(韩国允许使用7种,不允许使用5种)非营养性甜味剂。色谱分离在Xbridge BEH C18柱(3 mm×100 mm,2.5μm)上进行,采用梯度洗脱,流动相为水中的10 mM醋酸铵和甲醇中的10 mM醋酸铵。样品制备包括在分析前进行简单稀释、匀浆、离心并用C18柱净化。所有甜味剂的相对基质效应(%ME)在±20%以内。该方法还显示出良好的线性(R>0.99)。样品中的检测限和定量限分别在0.02 - 2.66和0.06 - 8.05 mg/kg范围内。三个浓度水平的回收率在80%至119%之间,相对标准偏差值低于10%。此外,确定的5种不同食品基质中12种甜味剂的扩展不确定度被确认为<14%。最后,该方法成功应用于对在韩国、澳大利亚和土耳其购买的681份食品样品中甜味剂的分析。这些结果表明该方法适用于同时测定各种食品中的多种甜味剂。