摘要
目的评价单色聚焦-能量色散X射线荧光光谱法测定粮食中硒含量的适用性。方法连续独立测定20个空白样品中硒的含量,确定该方法的检出限和定量限;对9组含不同浓度硒的大米、小麦、玉米质控样品及15组含不同浓度硒的糙米、小麦、玉米定值样品进行检测,确定方法的准确性和台间差;重复7次检测含中等浓度硒的质控样品及定值样品和连续12 h检测含中等浓度硒的质控样品及定值样品,确定方法的重复性和稳定性。结果该方法的检出限和定量限分别为0.013 mg/kg和0.044 mg/kg;质控样品检测结果均在赋值范围之内,定值样品测定结果与氢化物原子荧光光谱法测定结果无显著性差异。重复性、稳定性的标准差和极差以及台间差t检验值均符合LS/T 6402—2017《粮油检验设备和方法标准适用性验证及结果评价一般原则》的规定。结论该单色聚焦-能量色散X射线荧光光谱法能够准确检测稻谷、小麦、玉米样品中硒含量。
Objective To evaluate the applicability of monochromatic excitation-energy dispersive X-ray fluorescence spectrometry for determination of selenium in grain.Methods The content of selenium in 20 blank samples were detected to determine the limit of detection and limit of quantitation of the method.Totally 9 groups of rice,wheat and corn quality control samples with different concentrations of selenium and 15 groups of brown rice,wheat and corn fixed-value samples with different concentrations of selenium were tested,in order to get the accuracy and interstation difference of the method.Through 7 times of detection of quality control samples and fixed-value samples with middle concentration of selenium,and continuously detecting the same type of samples for 12 hours to assess the repeatability and stability of the method.Results The limit of detection and limit of quantitation of this method were 0.013 mg/kg and 0.044 mg/kg,respectively.The test results of the quality control samples were all within the assigned range and there were no significant differences between the measured value of the method and the value of hydride atomic fluorescence spectrometry.Meanwhile,the repeatability,standard deviation and range of stability,and inter-instrument agreement t-test values were in accordance with the regulations of LS/T 6402—2017 Inspection of grain and oils-The general principle of standard adaptability verification and evaluation results for equipments and testing methods.Conclusion This monochromatic focusing-energy dispersive X-ray fluorescence spectrometry can accurately detect the selenium content in rice,wheat and corn samples.
作者
彭志兵
胡春
左艳娜
国师榜
邱亦潇
况蔡萌
辛迪薇
PENG Zhi-Bing;HU Chun;ZUO Yan-Na;GUO Shi-Bang;QUI Yi-Xiao;KUANG Cai-Meng;XIN Di-Wei(Food Inspection and Testing Research Institute of Jiangxi General Institute of Testing and Certification,Nanchang 330052,China)
出处
《食品安全质量检测学报》
2025年第24期36-43,共8页
Journal of Food Safety and Quality
基金
2023年粮食行业标准制修订和标准品计划项目(国粮办[2023]252号)。
关键词
能量色散X射线荧光光谱法
单色聚焦
硒
粮食
适用性评价
energy dispersive X-ray fluorescence spectrometry
monochromatic excitation
selenium
grain
applicability evaluation
