摘要
目的:建立同时快速测定保健食品中阿伐那非、米罗那非、乌地那非、西地那非、他达拉非、沙格列汀和西布曲明等7种非法添加药物的超高效液相色谱-串联质谱检测方法。方法:试样前处理采用乙腈为提取溶剂,经超声处理,Waters ACQUITY UPLC®BEH C_(18)(100 mm×2.1 mm,1.7μm)色谱柱分离,以水(含0.1%甲酸)-乙腈(含0.1%甲酸)为流动相梯度洗脱,流速0.3 mL·min^(-1),柱温30℃,进样量2μL。质谱采用电喷雾离子源,以正离子多反应监测模式进行定性和定量分析。结果:7种非法添加药物在本方法色谱和质谱条件下8 min内能得到快速分离,在10~500 ng·mL^(-1)线性关系良好,相关系数R为0.9971~0.9992,检出限为0.0025 mg·kg^(-1)。结论:本方法前处理过程简单快速,选择性强,灵敏度高,能够快速、准确地同时对保健食品中非法添加的阿伐那非、米罗那非、乌地那非、西地那非、他达拉非、沙格列汀和西布曲明进行定性及定量测定。
Objective:To establish an UPLC-MS/MS method for simultaneous determination of avanafil,mirodenafil,udenafil,sildenafil,tadalafil,saxagliptin and sibutramine in health food.Method:Samples was extracted with acetonitrile and handled by ultrasound,used Waters ACQUITY UPLC®BEH column C_(18)(100 mm×2.1 mm,1.7μm)with mobile phase of water(contain 0.1%formic acid)and acetonitrile(contain 0.1%formic acid)by gradient elution;the flow rate was 0.3 mL·min^(-1),the column temperature was 30℃,and the sample volume was 2μL.ESI(electro spray ion source)was used for mass spectrometry,and positive ion multiple reaction monitoring mode was used for qualitative and quantitative analysis.Result:Seven illegally added drugs can be separated rapidly in 8 minutes under the conditions of this method,each component has a good linear relationship within the range of 10~500 ng·mL-1,the correlation coefficient R was between 0.9971 and 0.9992,the detection limit was 0.0025 mg·kg^(-1).Conclusion:The pretreatment process of this method is simple and rapid,high selectivity,high sensitivity,it can be used as a rapid and simultaneous determination method for the illegally addition of avanafil,mirodenafil,udenafil,sildenafil,tadalafil,saxagliptin and sibutramine in health food.
作者
吴芳海
许琨琨
卢文斌
王晓峰
蔡振世
WU Fanghai;XU Kunkun;LU Wenbin;WANG Xiaofeng;CAI Zhenshi(Quanzhou Institute for Food and Drug Control,Quanzhou 362000,China)
出处
《食品安全导刊》
2023年第12期112-116,共5页
China Food Safety Magazine
基金
福建省市场监督管理局科技项目(FJMS2021034)。
