HILIC-MS/MS Method for Analysis of Ephedrine in Internet-available Drugs
2017
Tircova, Barbora | Kozlik, Petr
A new separation method involving hydrophilic interaction liquid chromatography with tandem mass spectrometric detection has been developed for the analysis of ephedrine in a pharmaceutical solid dosage form. The optimized conditions for the analysis of ephedrine consisted of an Acquity BEH Amide column, and a mobile phase composed of acetonitrile/5 mM ammonium formate, pH 3.0, 88/12 (v/v), flow rate 0.4 mL min⁻¹ and column temperature 30 °C. The developed analytical procedure provides high throughput of samples where LC analysis takes only 90 s. Detection was performed by tandem mass spectrometry using electrospray ionization in multiple reaction monitoring mode. This method was found to be precise, linear, accurate, sensitive, selective and robust for routine application in screening of commercial pharmaceutical products based on the content of ephedrine. Application of the method for the determination of ephedrine content in 20 different pharmaceutical drug products revealed that 5 samples did not contain any ephedrine at all, 3 samples contained lower dosage than declared, and the dosage in 1 sample was exceeded.
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