Oasis MCX柱-高效液相色谱/三重四极杆质谱联用法测定火锅底料中罂粟壳不确定度评定

Uncertainty evaluation of determination of poppy shell in hot pot condiment by Oasis MCX column-high performance liquid chromatography/triple quadrupole mass spectrometry

目的评定Oasis MCX柱-高效液相色谱/三重四极杆质谱联用法测定火锅底料中罂粟壳不确定度。方法用Oasis MCX柱法对样品进行前处理,采用高效液相色谱/三重四极杆质谱联用法测定火锅底料中可待因、蒂巴因、吗啡、那可丁含量,并根据建立的数学模型对各分量进行不确定度评定。结果当火锅底料中可待因含量为43.1μg/kg时,扩展不确定度为5.4μg/kg(k=2);蒂巴因含量为4.63μg/kg时,扩展不确定度为0.13μg/kg(k=2);吗啡含量为42.0μg/kg时,扩展不确定度为4.4μg/kg(k=2);那可丁含量为4.83μg/kg时,扩展不确定度为0.17μg/kg(k=2)。结论曲线拟合是标准不确定度的最主要来源,其次为重复性实验。

Objective To evaluate the uncertainty of determination of opium poppy shell in hot pot condiment by Oasis MCX column-high performance liquid chromatography/triple quadrupole mass spectrometry.Methods The samples were pretreated by oasis MCX column method.The content of codeine,tibaine,morphine and nacotin in chafing dish was determined by high performance liquid chromatography/triple quadrupole mass spectrometry.According to the established mathematical model,uncertainty of each component was evaluated.Results When the codeine content in hot pot base was 43.1μg/kg,the expanded uncertainty was 5.4μg/kg(k=2);when the thebaine content was 4.63μg/kg,the expanded uncertainty was 0.13μg/kg(k=2);when the morphine content is 42.0μg/kg,the expanded uncertainty was 4.4μg/kg(k=2);when the noscapine content was 4.83μg/kg,the expanded uncertainty was 0.17μg/kg(k=2).Conclusion Curve fitting is the main source of standard uncertainty,followed by repeated experiments.