The objective of this study was to establish a novel method for rapid detection of six glucocorticoids (prednisone, prednisone acetate, prednisolone, hydrocortisone, hydrocortisone acetate, and dexamethasone) added illegally in dietary supplements simultaneously by combining thin layer chromatography (TLC) with spot-concentrated Raman scattering (SCRS). The doping ingredients were separated by TLC, and viewed and located with UV light (254 nm), enriched by chromatography, then Raman spectra were directly detected by a Raman Imagine microscope with 780 nm laser source. This method had complementary advantages of TLC and Raman spectroscopy, which enhanced the specificity of the test results. The limit of detection (LOD) of the reference substances were 4 μg, 4 μg, 4 μg, 6 μg, 6 μg, and 4 μg, respectively. The method was used to study the six glucocorticoids added illegally in five dietary supplements. Fake drugs had been detected. The study showed that the TLC-SCRS method is simple, rapid, specific, sensitive, and reliable. The method could be used for effective separation and detection of six chemical components used in dietary supplement products, and would have good prospects for on-site qualitative screening of dietary supplement products for adulterants.

A method for identifying six estrogen preparations by thin-layer chromatography combined with Raman imaging microscopy (TLC-RIM) was established. An appropriate pretreatment method was adopted to extract and purify the six estrogen preparations. After that, each estrogen extraction solution was spotted on a thin-layer chromatography plate. Estriol (E3), estradiol (E2), estradiol valerate (EV), estradiol benzoate (EB), nilestriol (CEE), and ethinylestradiol (EE2) were separated by TLC, and their R_f value and localization were determined under a UV lamp at 254 nm, followed by the in situ enrichment of the drug component. Using a 532 nm laser as the light source, the Raman scattering spectrum of the component was directly collected by micro-Raman imaging. The R_f values after TLC separation of the six estrogens and their Raman spectra can, respectively, reflect differences in polarity and structure, and they are not affected by the excipients of preparation. The detection limits of the six estrogens are 0.636, 1.00, 0.687, 0.497, 0.649, and 0.626 mg/mL. Based on the intensity of the minimum characteristic peak, the stability results within 40 min showed that the RSD of each substance is 1.34, 2.06, 1.65, 3.99, 1.16, and 2.71%, respectively. This method has strong specificity, good stability, and high sensitivity, and it can provide a new reference for improving the identification standards of estrogen preparations.