Abstract
An ultra-fast liquid chromatography-electrospray ionization tandem mass spectrometry method was developed and validated to simultaneously screen, confirm, and determine 18 illegal adulterants in herbal medicines and health foods for male sexual potency. The separation was achieved on a Shim-Pack XR-ODS II column (2.0 × 100 mm, 2.2 μm) with acetonitrile and aqueous solution (12 mmol/L ammonium formate, 0.01% acetic acid) as mobile phase at a flow rate of 0.4 mL/min with a gradient elution. The column temperature was maintained at 40°C and the run time was within 18 min. The 18 illegal adulterants were detected in electrospray ionization positive mode by multiple-reaction monitoring. All the calibration curves showed good linearity with correlation coefficient (r) higher than 0.996 within the tested concentration ranges. The extraction recoveries and relative recoveries were in the range of 79.5-114% and 82.0-120%, respectively. The RSD of repeatability and intermediate precision was all less than 18% and the accuracy was in the range of 81.7-118%. The intra-day and inter-day stability was in the range of 86.8-110%. The validated method was successfully applied to screen, confirm, and determine 16 samples. Nine products were confirmed to contain illegal adulterants and the contents of adulterants were related to the therapeutic dosages.
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