QuEChERS-超高液相色谱/串联质谱法测定炒白术中甲拌磷亚砜残留的不确定度评定  

Evaluation of Uncertainty in Determination of Phorate Sulfoxide Residues in Stir Fried Rhizoma Atractylodis by QuEChERS-ultra-high Liquid Chromatography/tandem Mass Spectrometry

作　　者：邹艺荣 洪家顺 Zou Yi-rong;Hong Jia-shun(Jiangxi Wantuo Environmental Testing Co,Ltd.,Shangrao Jiangxi 334000,China;Jiangxi Province evaluation and research center of daodi herbs,Nanchang Jiangxi 330029,China)

机构地区：[1]江西万拓环境检测有限公司,江西上饶334000 [2]江西省道地药材质量评价研究中心,江西南昌330029

出　　处：《江西化工》2023年第4期47-51,共5页Jiangxi Chemical Industry

摘　　要：目的:建立QuEChERS-超高液相色谱/串联质谱法测定药材中农药残留,并评定其不确定度。方法:按照《中国药典》2020版四部通则第五法测定药材中农药残留,评定不确定度。结论:对炒白术中农药残留不确定度评定影响最大的是农残对照品溶液配制,其次为仪器校准、回收率、样品重复性、样品称量、体积变化。通过对不确定度分量进行量化和合成,表明炒白术样品中甲拌磷亚砜残留为0.081mg/kg,扩展不确定度为0.005 mg/kg(k=2),该方法为科学评价QuEChERS-超高液相色谱/串联质谱法测定药材中农药残留的测量结果的准确性提供参考。Objective:to establish a QUECHERS-UPLC/ms/ms method for the determination of pesticide residues in medicinal materials and to evaluate its uncertainty.Methods:according to the fifth method of Chinese pharmacopoeia(2020 edition),the pesticide residues in medicinal materials were determined and the uncertainty was evaluated.Conclusion:the most influential factor on the uncertainty of pesticide residues in fried atractylodes macrocephala is the formulation of pesticide control solution,followed by instrument calibration,recovery,sample reproducibility,sample weighing,volume change.By quantifying and synthesizing the uncertainty components,the results showed that the residue of pho in Chinese fried atractylodes macrocephala was 0.081 mg/kg,and the expanded uncertainty was 0.005 mg/kg(K=2),this method provides a scientific reference for evaluating the accuracy of QUECHERS-UPLC/ms determination of pesticide residues in medicinal materials.

关 键 词：甲拌磷亚砜 炒白术 不确定度 超高液相色谱/串联质谱法 

分 类 号：O657.63[理学—分析化学] TS272.7[理学—化学]