摘要
目的建立液相色谱-离子阱-飞行时间质谱法(HPLC-IT-TOF-MS)测定中成药和保健食品中非法添加的格列波脲,并评定检出限的不确定度。方法通过对不确定度的来源进行分析,量化和合成,得出格列波脲检出限浓度的不确定度。结果扩展不确定度U=urel(X)×X×2=0.0037mg·L^(-1)(k=2),检出限可表示为:0.0063±0.0037mg·L^(-1)(k=2)。结论影响检出限测定结果的主要原因为标准溶液的配制、曲线拟合、测量重复性和方法回收率。
OBJECTIVE To establish a method for the determination glibornuride illegally added into Chinese Patent Drug and healthy food by high performance liquid chromatography-ion trap-time of flight mass spectrometry（HPLC-IT-TOF-MS）,and to evaluate the measurement uncertainty of the method detection limit. METHODS According to the relevant regulations,the sources of uncertainty that may be introduced were analyzed,quantified and combined. RESULTS The expended uncertainty of 0. 0037 mg·L^（-1）（k = 2） with 0. 0063 mg·L^（-1） of method detection limit of glibornuride was derived. CONCLUSION The configuration of standard solution,curve fitting,measurement repeatability and method recovery were the main sources of uncertainty.
作者
孙晶
曹玲
谭力
冯有龙
SUN Jing;CAO Ling;TAN Li;FENG You-long(Jiangsu Institute for Food and Drug Control, Nanjing 2!0008, Chin)
出处
《海峡药学》
2018年第5期50-53,共4页
Strait Pharmaceutical Journal
基金
国家科技支撑计划项目(2012BAK08B02)
关键词
HPLC-IT-TOF-MS
非法添加
格列波脲
检出限
不确定度
High performance liquid chromatography-ion trap-time of flight mass spectrometry （HPLC-IT-TOF-MS）
Illegal addition
Glibomuride
Limit of detection
Uncertainty evaluation
