缓解体力疲劳类保健食品中2种新的化学添加物的鉴定及含量检测

Identification and determination of 2 new added compounds in anti-fatigue health food

中文关键词:  超高效液相色谱-紫外-高分辨质谱联用仪  缓解体力疲劳  保健食品  促进剂DPG  促进剂M

英文关键词:ultra high performance liquid chromatograph–diode array detector-electrospray ion-quadrupole-time-of-flight mass spectrometer  anti-fatigue  health foods  accelerator DPG  accelerator M

中文摘要:

      目的 鉴定和检测缓解体力疲劳类保健食品中2种新的化学添加物的含量。方法 采用超高效液相色谱-紫外-超高分辨质谱联用检测方法, 利用ACQUITY UPLC?HSS T3(100 mm×2.1 mm, 1.8 μm)色谱柱, 以0.1%甲酸溶液和0.1%甲酸-乙腈梯度洗脱, 流速为0.3 mL/min。采用电喷雾离子源正离子模式(ESI+), 利用Q-TOF一级精密质量数推测分子式, 二级质谱碎片进一步确证结构。参照紫外吸收光谱, 并借助对照品进行确证, 利用Q-TOF一级精密质量数建立含量测定方法。结果 2种化学物质与其对照品在液相色谱分离保留时间、紫外吸收光谱、高分辨质谱中的一级母离子、二级碎片完全一致。对这2种化合物的分离、分析方法进行方法学验证, 线性范围内线性关系良好, 相关系数均大于0.990; 检出限为0.0012、0.057 ng, 回收率100%~102%, 相对标准偏差普遍小于3%。结论 本研究从14批缓解体力疲劳类保健食品中发现2种新的化学添加物, 并建立了液相-质谱的分析方法。

英文摘要:

      Objective To identify and test the content of 2 new chemical additives in health food for relieving physical fatigue. Methods The method of ultra high performance liquid chromatograph–diode array detector-electrospray ion-quadrupole-time-of-flight mass spectrometer used ACQUITY UPLC?HSS T3(100 mm× 2.1 mm, 1.8 μm) column with. 0.1% formic acid solution and 0.1% formic acid-acetonitrile gradient elution at a flow rate of 0.3 mL/min. The electrospray ionization ion source positive ion mode (ESI+) was used to predict the molecular formula by using the Q-TOF first order accurate mass number, level 2 pieces of mass spectrometry further confirmed the structure. According to the ultraviolet absorption spectrum, and confirmed with reference to the substance, the content determination method was established by using the first-class precision quality number of Q-TOF. Results The retention time of liquid chromatofraphy, ultraviolet absorption spectrum and the primary parent ion and secondary fragment in high resolution mass spectrometry of the two chemical substances were exactly the same as those of controls. The method for the separation and analysis of the two compounds were validated. The linear relationship in the linear range was good, and the correlation coefficient was greater than 0.990. The detection limit were 0.0012 ng and 0.057 ng, the recovery rate was 100%?102%, and the relative standard deviation was generally less than 3%. Conclusion In this study, two new chemical additives were found from 14 batches of health food for relieving physical fatigue, and a liquid-mass spectrometry analysis method was established.