保健食品中新型双醋酚汀衍生物的发现、合成与鉴定

目的:发现、制备和鉴定一种新型双醋酚汀衍生物。方法:在用超高效液相色谱—四级杆—飞行时间—质谱法对减肥类保健食品的日常筛查过程中，发现了一种疑似双醋酚汀的衍生物。经柱层析分离纯化得到该化合物，并通过同位素质谱图、二级质谱图、一维和二维核磁共振波谱图推测该化合物的可能结构。最终通过从头合成策略对所有可能结构进行制备，并将两种途径所得的产物进行谱图比对确证其精细结构。结果:该化合物为5-氯双醋酚汀[5-Cl oxyphenisatine di（acetate）]，是一种新型未见获批可作为食品添加剂的双醋酚汀衍生物。结论:该化合物的毒理药理学作用尚不明确，需引起监管机构的关注。掌握该类化合物的质谱裂解规律及可疑结构的从头合成将有利于新型化合物的精细结构确证。

Discovery, preparation and identification of a new type of oxyphenisatine di（acetate） analogue in dietary supplement

Objective: To find, prepare and identify a new oxyphenisatine di（acetate） analogue. Methods: A suspected derivative of oxyphenisatine di（acetate） was found by high-performance liquid chromatography-quadrupole-time-of-flight-mass spectrometry during the routine screening of weight loss healthcare product. The compound was isolated and purified by column chromatography, and the possible structures were inferred from the information of isotope mass spectra, secondary ion mass spectra, one-dimensional and two-dimensional NMR spectra. Finally, all possible structures were prepared by de novo synthesis strategy, and their fine structures were confirmed by spectral comparison. Results： The compound was identified as 5-Cl oxyphenisatine di（acetate）, a new type of oxyphenisatine di（acetate）, which has not been approved as food additives. Conclusion: The toxicological and pharmacological effects of this compound are not clear and should be of concern to regulators. The mass spectrometric fragmentation rule and the de novo synthesis of doubtful structures of these compounds will be beneficial to confirm the fine structure of new compounds.