title: Application of an ultrahigh-performance liquid chromatography coupled to quadrupole-orbitrap high-resolution mass spectrometry for the rapid screening, identification and quantification of illegal adulterated glucocorticoids in herbal medicines.
abstract: In this work, the ultrahigh-performance liquid chromatography quadrupole orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was applied to the rapid screening, identification and quantification of the illegal adulterated glucocorticoids in herbal medicines. The mass spectrometer was operated in positive ion mode and Full MS/dd-MS2(data-dependent MS2) mode, where selected ions were subjected to a dd-MS2scan with given fragmentation energy following a Full MS scan. The application of 70 000 FWHM mass resolution and narrow mass windows (5ppm) effectively improve the selectivity of the method, and a single injection was sufficient to perform the simultaneous screening and identification/quantification of 14 glucocorticoids in 15min. The method validation including selectivity, sensitivity, calibration curve, accuracy, precision, recovery, matrix effect and stability were evaluated. The results of all analytes showed excellent linear relationship while all coefficient of determination (r2) were>0.9990 over wide concentration ranges (e.g., 5-1000ng/mL for hydrocortisone butyrate, r2=1.0000). The recoveries were in the range of 86.1-102.7%, while the matrix effects ranged from 95.8%-105.8%. Accuracies and precisions were performed. The intra- and inter-day accuracies ranged from 90.6% to 108.9%, while the intra- and inter-day precisions were in the range of 0.5% to 8.5%. Finally, the established method was employed to detect illegal adulterated glucocorticoids in herbal medicines. It will provide more reliable technical basis for the drug quality supervision department and ensure public health.
authors: Key Laboratory of Natural Products Chemical Biology, Ministry of Education, School of Pharmaceutical Sciences, Shandong University, 250012 Jinan, PR China.
authors: Shuiqing
authors: S
authors: Zhou
authors: Shandong Institute for Food and Drug Control, 250101 Jinan, PR China.
authors: Changchuan
authors: C
authors: Guo
authors: Shandong Institute for Food and Drug Control, 250101 Jinan, PR China. Electronic address: shif250101@126.com.
authors: Feng
authors: F
authors: Shi
authors: School of Chemistry and Chemical Engineering, Shandong University, 250100 Jinan, PR China.
authors: Wei
authors: W
authors: Jiang
authors: Key Laboratory of Natural Products Chemical Biology, Ministry of Education, School of Pharmaceutical Sciences, Shandong University, 250012 Jinan, PR China. Electronic address: wangl-sdu@sdu.edu.cn.
authors: Lei
authors: L
authors: Wang
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003348:Cortisone / Q000031:analogs & derivatives / Q000032:analysis; D004340:Drug Contamination; D005938:Glucocorticoids / Q000032:analysis*; D057230:Limit of Detection; D010946:Plants, Medicinal / Q000737:chemistry*; D011241:Prednisone / Q000032:analysis; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D005938:Glucocorticoids; D003348:Cortisone; D011241:Prednisone
keywords: Glucocorticoid; Identification; Illegal adulteration; Orbitrap; Screening