QIAN Ye-fei, JIA Chang-ping, LU Hui, et al. Rapid Determination of 38 Glucocorticoids Illegally Added into Chinese Patent Medicines and Dietary Supplements by UPLC-MS-MS[J]. Chinese journal of experimental traditional medical formulae, 2016, 22(10): 60-66.
QIAN Ye-fei, JIA Chang-ping, LU Hui, et al. Rapid Determination of 38 Glucocorticoids Illegally Added into Chinese Patent Medicines and Dietary Supplements by UPLC-MS-MS[J]. Chinese journal of experimental traditional medical formulae, 2016, 22(10): 60-66. DOI: 10.13422/j.cnki.syfjx.2016100060.
Objective: To establish a rapid and accurate method for the determination of 38 glucocorticoids which were illegally added into the Chinese patent medicines and dietary supplements. Method: The ultra-performance liquid chromatography-tandem mass spectrum (UPLC-MS-MS) method was adopted on a Waters Acquity BEH-C18 (2.1 mm×50 mm
1.7 μm) column with 0.1% acetic acid acetonitrile solution (A)-0.1% acetic acid water solution (B) as the mobile phase for gradient elution at a flow rate of 0.3 mL·min-1
and the column temperature was 25℃. Electrospray ionization (ESI)
positive ion scanning and a multiple reaction monitoring (MRM) mode were used to quantitatively determine 38 glucocorticoids. The added chemical components were determined by comparing the molecular ion peaks
secondary fragment ion peaks
and retention time under MRM channels between sample peaks and reference peaks. The exact amount of added medicine was calculated according to the peak area of mass spectrometry with external standard method. Result: Under the above chromatography and mass spectrometry conditions
38 glucocorticoids were well separated. The limits of detection (LOD) and the limits of quantitation (LOQ) of this method were in the range of 0.3-1.6 μg·L-1 and 1.0-5.4 μg·L-1respectively. The recovery rates were in the range of 80.9%-119.4%. Conclusion: This method is simple
accurate
and highly sensitive
which can be used for the determination of illegally added glucocorticoids in Chinese patent medicines and dietary supplements.