Simultaneous Determination of Multi-Class Active Pharmaceutical Ingredients by UHPLC-HRMS
May 2021
in “
Journal of pharmaceutical and biomedical analysis
”
UHPLC-HRMS quadrupole-orbitrap mass spectrometer active pharmaceutical ingredients acne hair loss male erectile dysfunction skin whitening ultrasound-assisted extraction high-resolution product ion spectral library collision energies HRMS2 spectra stable isotopically labeled API analogs internal standards instrument quality control high-resolution mass spectrometry API UAE HRMS2 isotopically labeled standards quality control
TLDR A new method was developed to accurately detect and measure 47 different drug ingredients in various products.
A UHPLC-HRMS method using a quadrupole-orbitrap mass spectrometer was developed to detect and quantify 47 active pharmaceutical ingredients (APIs) commonly found in products for acne, hair loss, male erectile dysfunction, and skin whitening. The method included a fast ultrasound-assisted extraction (UAE) without sample cleanup and a high-resolution product ion spectral library for compound verification. Optimized collision energies ensured proper fragmentation of analytes, resulting in high HRMS2 spectra matching scores (0.6 or above). Eleven stable isotopically labeled API analogs served as internal standards and instrument quality control. The method was applied to analyze 100 products with complex matrices, successfully identifying 8 APIs in 26 products, with concentrations ranging from 103 μg/g to 156,000 μg/g.
