摘要
依据JJF 1059.1-2012《测量不确定度评定与表示》和CNAS-GL06-2019《化学分析中不确定度的评估指南》中不确定度评定的基本程序,通过建立数学模型,建立了高效液相色谱串联质谱法测定火锅食品中吗啡、可待因、罂粟碱、那可丁和蒂巴因含量不确定度的分析方法。结果表明,罂粟碱、那可丁、蒂巴因、吗啡、可待因合成标准不确定度的最终结果分别为5.1×10-2,5.0×10-2,5.8×10-2,8.4×10-2,8.5×10-2;影响测量结果不确定度的主要因素是样品回收率,样品平行试验重复性,样品提取,校准曲线拟合,标准工作溶液的配置。从校准曲线拟合这一不确定度分量可以看出,采用内标法进行测定的吗啡和可待因明显优于外标法测量的其他3种物质,可通过内标法进行测定,以降低样品基质不同所引入的不确定度。
According to the procedure for uncertainty assessment described in JJF 1059.1-2012 "Evaluation of uncertainty in chemical analysis measurement" and CNAS-GL06-2019"Guidance on evaluating the uncertainty in chemical analysis",a mathematical model was established,and an analytical method for the determination of uncertainty of morphine,codeine,papaverine,narcotine and thebaine in chafing dish food by LC-MS/MS was established.The results showed that the synthesis of relative standard uncertainty for papaverine,narcotine,thebaine,morphine and codeine were 5.1×10-2,5.0×10-2,5.8×10-2,8.4×10-2,and 8.5×10-2,respectively;the main factors affecting the uncertainty of measurement results included the sample recovery rate,the repeatability of parallel experiments,sample extraction,calibration curve fitting,and the configuration of standard working solution.From the uncertainty component of calibration curve fitting,it was revealed that morphine and codeine determined by the internal standard method were obviously superior to the other three substances measured by the external standard method.Consequently,using the internal standard method could reduce the uncertainty caused by different sample matrices.
作者
卫星
李小红
董曼曼
孙晓
张荻悦
张亚锋
WEI Xing-hua;LI Xiao-hong;DONG Man-man;SUN Xiao;ZHANG Di-yue;ZHANG Ya-feng(Xi’an Institute for Food and Drug Control, Xi’an, Shaanxi 710054, China)
出处
《食品与机械》
北大核心
2019年第8期77-82,154,共7页
Food and Machinery
基金
陕西省科技厅科技统筹创新工程计划项目(编号:2014FWPT-01)
作者简介
卫星华,女,西安市食品药品检验所工程师,硕士;通信作者:张亚锋(1978-),男,西安市食品药品检验所副主任药师,硕士。E-mail:yafeng@163.com.
