超高效液相色谱法测定酒精饮料中非法添加抗疲劳药物他达拉非及2种类似物
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, 1.8 μm)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0.6、0.6、0.5 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1.5%、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 0.6, 0.6, and 0.5 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 1.5%, 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.
标题：超高效液相色谱法测定酒精饮料中非法添加抗疲劳药物他达拉非及2种类似物
英文标题：Determination of illegally added antifatigue drugs tadalafil and 2 analogues in alcoholic beverage by ultra performance liquid chromatography
作者：
谢强胜 山东省食品药品检验研究院
王慧 中国食品药品检定研究院
张子璇 利兹大学
王坤 山东省食品药品检验研究院
李启艳 山东省食品药品检验研究院
胡德福 山东省食品药品检验研究院
中文关键词: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,
英文关键词:ultra performance liquid chromatography,illegal addition,antifatigue drugs,tadalafil,alcoholic beverage,
发表日期：2017-02-15
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