Rapid Determination of 12 Kinds of Illegally Added Drugs in Throat-clearing Healthcare Food Products by UPLC-Q/Orbitrap HRMS
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Abstract:
A method for rapid screening and quantitative analysis of 12 kinds of illegally added drugs in throat-cleaning healthcare food products based on ultra high performance liquid chromatography-quadrupole/elecrostatic orbitrap high resolution mass spectrometry (UPLC-Q/Orbitrap HRMS) was developed. The sample was extracted with acetonitrile and centrifuged at a high speed. The separation of the 12 target compounds was performed on a ZOBAX XDB-C18 column (50 mm × 2.1 mm, 1.8 μm) through a gradient elution with 0.1% formic acid (containing 5 mmol/L ammonium acetate) and methanol as the mobile phase. Mass spectrometry analysis was performed via the full MS/dd-MS2 acquisition with positive ionization mode, and the chromatographic peak areas obtained through extracting the accurate mass number of parent ions by full MS first-order mass spectrometry were quantified. A database was established for qualitative screening based on the retention time, primary precursor mass and secondary fragment ions information from DD-MS2 scans. The 12 kinds of drugs were effectively separated within 7.63 min with the mass accuracy deviation lower than 1.48×10-6. A good linearity was obtained in the range from 1.00 µg/L to 200.00 µg/L, with a correlation coefficients higher than 0.999. The lower limits of detection ranged from 50.00 µg/kg to 150.00 µg/kg. The average spiked recoveries for 12 target compounds were between 75.15% and 117.65%, with relative standard derivations (RSDs) ranged from 0.89% to 4.84%. The method was simple, fast, accurate, sensitive and selective, thus can be used for rapid qualitative screening and quantitative analysis of illegally added chemical drugs in throat-cleaning healthcare food products.
