title: Rapid on-site detection of ephedrine and its analogues used as adulterants in slimming dietary supplements by TLC-SERS.
abstract: Ephedrine and its analogues are in the list of prohibited substance in adulteration to botanical dietary supplements (BDS) for their uncontrollable stimulating side effects. However, they were always adulterated illegally in BDS to promote losing weight. In order to avoid detection, various kinds of ephedrine analogues were added rather than ephedrine itself. This has brought about great difficulties in authentication of BDS. In this study, we put forward for the first time a method which combined thin-layer chromatography (TLC) and surface-enhanced Raman scattering (SERS) to directly identify trace adulterant. Ephedrine, pseudoephedrine, methylephedrine, and norephedrine were mixed and used in this method to develop an analytical model. As a result, the four analogues were separated efficiently in TLC analysis, and trace-components and low-background SERS detection was realized. The limit of detection (LOD) of the four analogues was 0.01 mg/mL. Eight common Raman peaks (△υ = 620, 1003, 1030, 1159, 1181, 1205, 1454, 1603 cm(-1)) were extracted experimentally and statistically to characterize the common feature of ephedrine analogues. A TLC-SERS method coupled with common-peak model was adopted to examine nine practical samples, two of which were found to be adulterated with ephedrine analogues. Identification results were then confirmed by UPLC-QTOF/MS analysis. The proposed method was simple, rapid, and accurate and can also be employed to trace adulterant identification even when there are no available reference derivatives on-site or unknown types of ephedrine analogues are adulterated.
authors.affiliation: Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, 325 Guohe Road, Shanghai, 200433, China.
authors.forename: Diya
authors.initials: D
authors.lastname: Lv
authors.forename: Yan
authors.initials: Y
authors.lastname: Cao
authors.forename: Ziyang
authors.initials: Z
authors.lastname: Lou
authors.forename: Shujin
authors.initials: S
authors.lastname: Li
authors.forename: Xiaofei
authors.initials: X
authors.lastname: Chen
authors.forename: Yifeng
authors.initials: Y
authors.lastname: Chai
authors.forename: Feng
authors.initials: F
authors.lastname: Lu
mesh_terms: D002855:Chromatography, Thin Layer / Q000379:methods*; D019587:Dietary Supplements / Q000032:analysis*; D004340:Drug Contamination / Q000517:prevention & control; D004809:Ephedrine / Q000031:analogs & derivatives / Q000032:analysis*; D013059:Spectrum Analysis, Raman / Q000379:methods*
chemical_list: D004809:Ephedrine