超声提取-高效液相色谱法测定酱类制品中爱德万甜及其不确定度分析  

Determination of advantame in sauce products by ultrasonic extraction-high performance liquidchromatography and its uncertainty analysis

作　　者：黄惠敏 刘宁 段虎 杨光 HUANG Huimin;LIU Ning;DUAN Hu;YANG Guang(Luohe Product Quality Inspection and Testing Center,Luohe 462000,China)

机构地区：[1]漯河市产品质量检验检测中心,河南漯河462000

出　　处：《中国酿造》2024年第12期211-216,共6页China Brewing

基　　金：河南省市场监督管理局科技计划项目(2022sj63)。

摘　　要：该研究通过优化仪器检测条件,建立酱类制品中新型甜味剂爱德万甜的超声提取-高效液相色谱(HPLC)检测法,并通过建立数学模型,对标准溶液、标准曲线拟合、样品前处理、HPLC仪及测量重复性引入的不确定度进行分析。结果表明,酱类制品样品经超声提取后,经C18色谱柱(150 mm×4.6 mm,5μm)分离(柱温30℃),采用乙腈-水作为流动相进行梯度洗脱,激发波长为232 nm、发射波长为313 nm。在此检测条件下,爱德万甜保留时间为7.069 min,线性回归方程为y=1.64e+005x+2.74e+002,在0.05~5μg/m L的质量浓度范围内,线性关系良好,相关系数(R^(2))=0.999 8,检出限为0.25 mg/kg,定量限为0.625 mg/kg,加标回收率为91.2%~98.5%,精密度试验结果的相对标准偏差(RSD)为1.09%~2.48%,该方法提取简单,污染少,耗时短,灵敏度高,结果准确稳定,可适用于酱类制品中爱德万甜的测定。该方法不确定度的主要来源是标准曲线拟合(0.029 8),为检测过程中的关键控制点。The ultrasonic extraction-high performance liquid chromatography(HPLC)method for the detection of advantame in sauce products was established by optimizing instrument detection conditions.A mathematical model was established to analyze the uncertainties introduced by the standard solution,standard curve fitting,sample pretreatment,HPLC,and measurement repeatability.The results showed that after ultrasonic extraction,the sauce products sample was centrifuged,and separated on a C18 column(150 mm×4.6 mm,5μm)(column temperature 30℃)with acetonitrile-water as mobile phase for gradient elution.The excitation wavelength was 232 nm and the emission wavelength was 313 nm.Under these detection conditions,the retention time of advantame was 7.069 min,the linear regression equation was y=1.64e+005x+2.74e+002 with good linear relationship in the concentration range of 0.05-5μg/ml,the correlation coefficient(R^(2))was 0.9998,the limit of detection was 0.25 mg/kg,the limit of quantitation was 0.625 mg/kg,the recovery rate was 91.2%-98.5%,and the relative standard deviation(RSD)of the precision test results was 1.09%-2.48%.The method had the advantages of simple extraction,less pollution,short time,high sensitivity,accurate and stable results,which could be applied to the determination of advantame in sauce products.The main source of uncertainty in the method was the standard curve fitting(0.0298),which was a key control point in the detection process.

关 键 词：超声提取 高效液相色谱法 酱类制品 爱德万甜 不确定度 

分 类 号：O657.72[理学—分析化学]