摘要
目的:建立缓解体力疲劳类保健食品中非法添加四种新型他达拉非衍生物的检测方法并考察其可行性。方法:筛选出具有相同结构的四种新型他达拉非衍生物,建立液相色谱法初筛与定量(以富士C18-4.6×250mm-5μm为色谱柱,以乙腈-0.1%三氟乙酸水为流动相梯度洗脱,并于230nm波长下采集信号,以DAD光谱图初步定性、外标法定量)和液质联用法确证(以含0.1%乙酸的0.02mol/L乙酸铵溶液-乙腈-甲醇(45∶25∶30)为流动相等度洗脱,选择电喷雾电离源ESI+扫描,通过比较样品与对照品的分子离子峰、二级碎片离子峰进行确证)的检测方法,并在常见的饮料、酒剂、片剂、胶囊、咖啡、软胶囊和口服液7种基质中对标准曲线相关系数、线性范围、重复性、回收率、定量限、检出限等方法学参数进行考察。结果:四种新型他达拉非衍生物质量浓度在0~80μg/mL内与峰面积有良好的线性关系,对7种不同基质分别进行三个浓度水平的准确度评价,平均回收率均在90%~105%之间。结论:该方法具有快速、准确、高灵敏度等优点,可作为测定保健食品中非法添加四种新型他达拉非衍生物的有效方法。
Objective:To establish a determination method of four novel Tadalafil derivatives illegally added to foods supplements for fight fatigue and its feasible.Method:Four same structure Tadalafil derivatives were selected and liquid chromatography was used in the early screening stage.Quantitative detection was performed by Fuji C18-4.6×250mm-5μm chromatographic column at the condition of:acetonitrile-0.1%trifluoroacetic acid as mobile phase gradient elution,230nm wavelength,DAD spectrogram preliminary qualitative and quantitative analysis and external standard method.The determination method was also confirmed by liquid chromatography-mass spectrometry(LC-MS)in the condition of:0.1%acetic acid,0.02mol/L ammonium acetate solution-acetonitrile-methanol(45∶25∶30)isocratic elution,electrospray ionization source ESI+scan.By comparing molecular ion peaks of samples and reference substance,the secondary fragment ion peaks were identified.The method was tested in beverage,wine,tablet,capsule,coffee,soft capsule and liquid medicine total of 7 kinds of substance.The matrix of correlation coefficient of standard curve,linear range,repeatability,recovery,quantitative limit parameters,detection limit were investigated.Results:The concentration of four new Tadalafil derivatives in the range of 0~80 g/mL had a good linear relationship with the peak area;the accuracy of three concentration levels of seven different substrates was evaluated,average recovery was between 90%~105%.Conclusion:This method has the advantages of rapid,accurate and high sensitivity,and can be used as an effective method for the determination of four novel Tadalafil derivatives in food.
作者
王子龙
梁卜文
董培智
刘文博
王珂
项新华
WANG Zi-long;LIANG Bu-wen;DONG Pei-zhi;LIU Wen-bo;WANG Ke;XIANG Xing-hua(Shanxi Institute for Food and Drug Control,Taiyuan 030031;Shanxi University of Traditional Chinese Medicine,Jinzhong 030619;China Food and Drug Testing Institute,Beijing 102629)
出处
《中国食品添加剂》
CAS
北大核心
2021年第1期64-71,共8页
China Food Additives
基金
山西省重点研发计划项目(201903D321011)。
关键词
保健食品
他达拉非衍生物
新型非法添加化合物
方法建立
health food
derivatives of tadalafil
new illegal addition of compounds
method to establish
作者简介
王子龙(1987-),男,学士,中级工程师,研究方向:食品药品检验及质量研究;通讯作者:项新华(1970-),男,硕士,主任技师,研究方向:食品药品检测质量管理。
