超高效液相色谱-质谱联用法测定保健食品中的米罗那非和庆地那非  

Determination of Mirodenafil and Gendenafil in the Heathy Food by UPLC-MS

作　　者：王凤芹 张淮光 张秋妍 李子华 WANG Fengqin;ZHANG Huaiguang;ZHANG Qiuyan;LI Zihua(Fuyang Inspection and Testing Center,Fuyang 236111,China;School of Biological and Food Engineering,Fuyang Normal University,Fuyang 236037,China)

机构地区：[1]阜阳市食品药品检验检测中心,安徽阜阳236111 [2]阜阳师范大学生物与食品工程学院,安徽阜阳236037

出　　处：《食品安全导刊》2024年第28期51-58,共8页China Food Safety Magazine

基　　金：安徽省市场监督管理局科技计划项目(2023MK023)。

摘　　要：建立超高效液相色谱-质谱联用法测定缓解疲劳保健食品中非法添加米罗那非、庆地那非含量的检测方法。在电喷雾离子源正模式多反应监测方式下,以米罗那非定量/定性子离子对99.1/296.1,庆地那非定量/定性子离子对285.2/327.1为目标监测离子,空白基质外标法定量。结果:空白基质无干扰;米罗那非、庆地那非在10~1000 ng·mL^(-1)线性关系良好,相关系数分别为0.9997和0.9993;米罗那非的方法精密度为1.5%,平均回收率为90.4%~97.9%,相对标准偏差为0.9%~1.8%;庆地那非的方法精密度为1.2%,平均回收率为89.4%~96.6%,相对标准偏差为0.6%~2.4%;两者方法检出限、定量限分别为50μg·kg^(-1)和100μg·kg^(-1)。本文所建立的方法专属性强、准确、灵敏,可作为缓解疲劳类保健食品中非法添加米罗那非、庆地那非的痕量分析方法。To establish a method for determination of mirodenafil and gendenafil illegally added in the relieve fatigue heathy food by UPLC-MS.Mirodenafil quantitive product ion 99.1 and qualitative product ion 296.1,gendenafil quantitive product ion 285.2 and qualitative product ion 327.1 were detected as target ions under the positive mode multiple reaction monitoring,and quantitative analysis used blank matrix external standard method.The results indicated that the blank matrix solution had no interference.Milonafil and gendenafil had a good linear relationship within the range of 10~1000 ng·mL^(-1),with a correlation coefficient of 0.9997 and 0.9993,respectively.The precision of the method for mironafine is 1.5%,average recovery rates were from 90.4%to 97.9%,and the relative standard deviation were between 0.9%to 1.8%.The precision of the method for gendenafil is 1.2%,average recovery rates were between 89.4%to 96.6%,with relative standard deviation of 0.6%to 2.4%.The method detection limit and quantification limit are 50μg·kg^(-1)and 100μg·kg^(-1),respectively.The method is high specificity,accurate and sensitive,can be used as a trace analysis method for illegally adding mirodenafil and gendenafil in fatigue relieving health foods.

关 键 词：米罗那非 庆地那非 超高效液相色谱-质谱联用法(UPLC-MS) 保健食品 非法添加 

分 类 号：TS218[轻工技术与工程—粮食、油脂及植物蛋白工程] O657.63[轻工技术与工程—食品科学与工程]