Simultaneous analysis of 23 illegal adulteratedaphrodisiac chemical ingredients in health foodsand Chinese traditional patent medicines byultrahigh performance liquid chromatographycoupled with quadrupole time-of-flight massspectrometry

This paper presents an application of ultra high-performance liquid-chromatographyquadrupole-TOF high resolution mass spectrometry (UHPLC-Q-TOF HRMS) for simultaneousanalysis of 23 illegal adulterated aphrodisiac type chemical ingredients in healthfoods and Chinese Traditional Patent Medicines (CTPMs). The mass spectrometer wasoperated in Information Dependent Acquisition (IDA) mode, which provides crucial informationfor the elemental composition analysis, structure elucidation and quantitativeanalysis simultaneously. Quantitative analysis was performed using the peak areas of theprecursor ions in the XICs. The method validation included assessment of selectivity,sensitivity, calibration curve, accuracy, precision, recovery, matrix effect and stability. Theresults show good linear relationship with the concentrations of the analytes over wideconcentration ranges (e.g., 0.05e10 mg/g for sildenafil) as all the fitting coefficients ofdetermination r2 are >0.9984. The detection limits (LODs) were in the range of 0.002e0.1 mg/g. The recoveries were able to reach 82.5e103.6%, while the matrix effects ranged from 87.7to 109.3%. The intra- and inter-day accuracies were in the range of 82.3e113.8%, while theintra- and inter-day precision ranged from 0.4 to 13.6%. Among 40 batches of health foodsand 32 batches of CTPMs (including 28 capsules, 32 tablets, 10 liquid and 2 pills) samples, 28batches 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.