Shandong Institute for Food and Drug Control, Jinan, China.
Dong-E E-jiao Co., Ltd, National Engineering Technology Research Center of Gelatin Medicine, Shandong Province Key Laboratory of R&D of the Gelatin Medicine, Liaocheng, China.
J Food Drug Anal. 2018 Jul;26(3):1138-1153. doi: 10.1016/j.jfda.2018.02.003. Epub 2018 Mar 14.
This paper presents an application of ultra high-performance liquid-chromatography-quadrupole-TOF high resolution mass spectrometry (UHPLC-Q-TOF HRMS) for simultaneous analysis of 23 illegal adulterated aphrodisiac type chemical ingredients in health foods and Chinese Traditional Patent Medicines (CTPMs). The mass spectrometer was operated in Information Dependent Acquisition (IDA) mode, which provides crucial information for the elemental composition analysis, structure elucidation and quantitative analysis simultaneously. Quantitative analysis was performed using the peak areas of the precursor ions in the XICs. The method validation included assessment of selectivity, sensitivity, calibration curve, accuracy, precision, recovery, matrix effect and stability. The results show good linear relationship with the concentrations of the analytes over wide concentration ranges (e.g., 0.05-10 μg/g for sildenafil) as all the fitting coefficients of determination r are >0.9984. The detection limits (LODs) were in the range of 0.002-0.1 μg/g. The recoveries were able to reach 82.5-103.6%, while the matrix effects ranged from 87.7 to 109.3%. The intra- and inter-day accuracies were in the range of 82.3-113.8%, while the intra- and inter-day precision ranged from 0.4 to 13.6%. Among 40 batches of health foods and 32 batches of CTPMs (including 28 capsules, 32 tablets, 10 liquid and 2 pills) samples, 28 batches of heath foods were positive. The detected chemical ingredients involved sildenafil, tadalafil, aildenafil and sulfoaildenafil. This method can be used for the screening, identification and quantification of illegal adulterated aphrodisiac chemical ingredients in health foods and CTPMs. Moreover, the LC-Q-TOF MS is very useful to structural elucidation of unknown compound.
本文应用超高效液相色谱-四级杆飞行时间高分辨质谱（UHPLC-Q-TOF HRMS）同时分析保健品和中药传统方剂中 23 种非法掺假壮阳类型化学成分。质谱仪以信息依赖性采集（IDA）模式运行，为元素组成分析、结构阐明和定量分析同时提供关键信息。定量分析采用 XIC 中前体离子峰面积进行。方法验证包括选择性、灵敏度、校准曲线、准确性、精密度、回收率、基质效应和稳定性评估。结果表明，在宽浓度范围内（例如，西地那非为 0.05-10μg/g），分析物的浓度与峰面积之间具有良好的线性关系，所有拟合系数 r 均>0.9984。检测限（LOD）范围为 0.002-0.1μg/g。回收率能够达到 82.5-103.6%，而基质效应范围为 87.7-109.3%。日内和日间准确度范围为 82.3-113.8%，而日内和日间精密度范围为 0.4-13.6%。在 40 批保健品和 32 批中药（包括 28 粒胶囊、32 片、10 液体和 2 丸）样品中，28 批保健品呈阳性。检测到的化学成分包括西地那非、他达拉非、阿伐那非和磺酰基艾地那非。该方法可用于保健品和中药中非法掺假壮阳化学成分的筛选、鉴定和定量分析。此外，LC-Q-TOF MS 非常有助于未知化合物的结构阐明。
