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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 an HPLC method for the determination of tadalafil and two analogues in alcoholic beverages. Methods The detection wavelength was 290 nm and the flow rate was 0.3 mL / min with a Agillent Zorbax SB-C18 column (2.1 mm × 50 mm, 1.8 μm). The mobile phase A was 0.1% ammonium acetate solution (pH = 3.4), mobile phase B acetonitrile, according to a gradient elution. Results Tadalafil, demethylated tadalafil and tadalafil showed good linearity in the range of 0.6-120, 0.493-98.6 and 0.56-112 mg / L, respectively. The detection limits were 0.06, The average recoveries were 101.8%, 101.8% and 101.7%, respectively, with RSDs of 1.51%, 0.87% and 0.64%, respectively n = 6). Conclusions This method is simple in pre-treatment, short in analysis time, high in sensitivity and good in reproducibility. It can be used for the detection of anti-fatigue chemicals illegally added to alcoholic beverages.