高分辨四级杆串联飞行时间质谱快速鉴定一种他达拉非衍生物

Identification of a Tadalafil Analogue Based on Q-TOF-MS

目的鉴定保健食品中非法添加的他达拉非类似物。方法样品采用C18色谱柱分离,以0.1%甲酸溶液和乙腈梯度脱,利用高分辨四级杆串联飞行时间质谱(Q-TOF-MS),核磁共振(NMR)确证结构。结果运用HPLC-DAD,Q-TOF-MS及NMR鉴定出该化合物的结构,化学名为(6S,12aR)-6-(1,3-苯并二氧戊环-5)-2-羟乙基-2,3,6,7,12,12a-六氢吡嗪并[1',2'∶1,6]吡啶并[3,4-b]吲哚-1,4-二酮。结论利用Q-TOF-MS确证在保健食品中检出该他达拉非衍生物的结构,本实验可以为快速鉴定保健食品或非药品冒充药品中非法添加此类衍生物提供借鉴。

OBJECTIVE To identify a new tadalafil analogue illegally adulterated in health foods. METHODS The sam- ples were separated by C^s chromatographic column using gradiet elution with 0. 1% formic acid solution and acetonitrile, and the detection was performed using quadrupole time-of-flight mass spectrometry（Q-TOF/MS） and nuclearmagnetic resonance（NMR）. RESULTS The chemical structure of the new compound was elucidated by HPLC, LC-Q-TOF/MS, and NMR as（6S, 12aR）- 6-（1,3-benzodioxol-5-yl） -2,3,6,7,12,12a-hexahydro-2-（2-hydroxyethyl） -pyrazino [ 1 ＇2＇ ： 1,6 ] pyrido [ 3,4-b ] indole-1,4- dione. CONCLUSION By using Q-TOF-MS, the structure of the tadalafil analogue illegally adulterated in health foods is dis- closed for the first time. The method can be used for rapid detection of unknown novel analogues illegally added in health foods or non-pharmaceutical products.