降糖类口服液甲苯磺丁脲等5种非法添加物基体标准物质的研制  

Development of Matrix Reference Material of 5 Illegal Additives Such As Tolbutamide in Hypoglycemic Oral Liquid

作　　者：时玲 国振[1] 赵光亮 李秀琴[1] 张庆合[1] SHI Ling;GUO Zhen;ZHAO Guang-liang;LI Xiu-qin;ZHANG Qing-he(Division of Chemical Metrology and Analytical Science,National Institute of Metrology,Beijing 100029,China)

机构地区：[1]中国计量科学研究院化学计量与分析科学研究院,北京100029

出　　处：《化学试剂》2022年第12期1824-1829,共6页Chemical Reagents

基　　金：国家市场监督管理总局科技计划资助项目(2021MK156);中央级公益性科研院所基本科研业务费资助项目(AKYZZ2117);婴幼儿配方奶粉中维生素等标准物质研制资助项目(AKYZZ2219)。

摘　　要：采用添加法制备了降糖类口服液中甲苯磺丁脲、马来酸罗格列酮、格列本脲、格列喹酮和瑞格列奈基体标准物质候选物;建立了高效液相色谱方法准确定值方法,甲苯磺丁脲、马来酸罗格列酮、格列本脲、格列喹酮、瑞格列奈的加标回收率分别为100.3%~104.8%、94.4%~102.9%、97.7%~102.7%、96.2%~103.7%、96.6%~103.1%,RSD依次为1.0%~3.1%、0.9%~1.8%、0.6%~1.0%、1.0%~1.9%、0.8%~1.6%。标准物质均匀性和稳定性均良好。并对该标准物质的不确定度进行系统评估,定值结果为:甲苯磺丁脲(63.6±1.1)mg/kg、马来酸罗格列酮(42.2±1.2)mg/kg、格列本脲(22.6±0.7)mg/kg、格列喹酮(19.7±0.6)mg/kg、瑞格列奈(60.0±1.5)mg/kg,扩展因子k=2。该标准物质可用于食品检测实验室相关项目的方法开发、日常检测质量控制以及实验室能力验证等领域,保证实验室检测数据质量,提升检测能力。This study developed matrix reference material(RM)candidates of tolbutamide,rosiglitazone maleate,glibenclamide,gliquidone,and repaglinide in hypoglycemic oral liquid using an additive method.A high performance liquid chromatography(HPLC)method for determining quasi-deterministic values was established.The spiked recoveries of tolbutamide,rosiglitazone maleate,glibenclamide,gliquidone and repaglinide were 100.3%~104.8%,94.4%~102.9%,97.7%~102.7%,96.2%~103.7%and 96.6%~103.1%,respectively,with corresponding RSDs of 1.0%~3.1%,0.9%~1.8%,0.6%~1.0%,1.0%~1.9%,0.8%~1.6%.The reference materials have good homogeneity and stability.The uncertainties of the RM candidates were systematically evaluated to be:tolbutamide(63.6±1.1)mg/kg,rosiglitazone maleate(42.2±1.2)mg/kg,glibenclamide(22.6±0.7)mg/kg,gliquidone(19.7±0.6)mg/kg,and repaglinide(60.0±1.5)mg/kg,with an extension factor k=2.The RMs developed could be applied in methods development,quality control,and verification for food testing laboratories to improve accuracy and enhance measurement capability.

关 键 词：降糖类口服液 标准物质 非法添加物 高效液相色谱法 不确定度评估 

分 类 号：O652.1[理学—分析化学]