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_附件.docVIP

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 谢强胜1#, 王 慧2#, 张子璇3, 王 坤1, 李启艳1, 胡德福1* (1. 山东省食品药品检验研究院, 济南 250101; 2. 中国食品药品检定研究院, 北京 100050;3. 利兹大学, 利兹 LS29JT) 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, 1.8 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(RSDs)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。 关键词 Determination of illegally added antifatigue drugs tadalafil and 2 analogues in alcoholic beverage by ultra performance liquid chromatography XIE Qiang-Sheng1#, WANG Hui2#, ZHANG ZI-Xuan3, WANG Kun1, LI Qi-Yan1, HU De-Fu1* (1. Shandong Institute for Food and Drug Control, Jinan 250101, China; 2. Naional Institutes for Food and Drug Control, Beijing 100050, China; 3. University of Leeds, Leeds LS29JT, UK) ABSTRACT: 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 simpl