摘要
目的建立超高效液相色谱法测定酒饮料中他达拉非和2种类似物的分析方法。方法采用Agillent Zorbax SB-C18(2.1 mm×50 mm,1.8μm)色谱柱,二极管阵列检测器,检测波长为290 nm,流速为0.3 mL/min,流动相A为0.1%乙酸铵溶液(pH=3.4),流动相B为乙腈,按梯度进行洗脱。结果氨基他达拉非、去甲基他达拉非、他达拉非分别在0.6~120、0.493~98.6、0.56~112 mg/L范围内呈现良好的线性关系,检出限分别是0.06、0.06、0.05 ng,方法精密度分别为0.92%、1.1%、0.68%(n=6),平均回收率分别为101.8%、101.8%、101.7%,RSD分别为1.51%、0.87%、0.64%(n=6)。结论该方法前处理简单、分析时间短、灵敏度高、重现性好,可用于抗疲劳类化学药物在酒精饮料中非法添加的检测。
Objective To establish a method for the determination of tadalafil and other 2 analogues（amino tadalafil and dimethyl tadalafil） in alcoholic beverage by ultra performance liquid chromatography（UPLC）.Methods Agilent Zorbax SB-C18 column（2.1 mm×50 mm,1.8 μm） was used with a mobile phase consisting of acetonitrile and 0.01 mol/L ammonium acetate（pH=3.4） by gradient elution at a flow rate of 0.3 mL/min.The illegally added antifatigue drugs were detected by a photodiode array detector.The detection wavelength was set at 290 nm.Results The linearity ranges of amino tadalafil,dimethyl tadalafil and tadalafil were 0.6～120,0.493～98.6,and 0.56～112 mg/L,respectively.The limits of determination were 0.06,0.06,and 0.05 ng and the precisions of the method（RSDs） were 0.92%,1.1% and 0.68%（n=6）,respectively.The average recoveries were 101.8%,101.8% and 101.7%（n=6） and the RSDs were 1.51%,0.87% and 0.64%（n=6）,respectively.Conclusion The established method has the advantages of simple sample pre-treatment,rapid detection,satisfactory recovery and good reproducibility,which is suitable for the determination of illegally added antifatigue drugs in alcoholic beverage.
出处
《食品安全质量检测学报》
CAS
2017年第3期1030-1036,共7页
Journal of Food Safety and Quality
关键词
超高效液相色谱法
非法添加
抗疲劳药物
他达拉非
酒精饮料
ultra performance liquid chromatography
illegal addition
antifatigue drugs
tadalafil
alcoholic beverage
