Determination of selected biogenic amines in Acacia rigidula plant materials and dietary supplements using LC–MS/MS methods

Pawar, Rahul S.; Grundel, Erich; Fardin‐Kia, Ali Reza; Rader, Jeanne I.

doi:10.1016/j.jpba.2013.09.012

Cited by 58 publications

(88 citation statements)

References 22 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Then, their peak intensity was used to calculate the relative standard deviation (RSD) value to Table S1). The precision of SERS is not as good as LC-MS or GC-MS [33].…”

Section: Analysis Of the Common And Characteristic Peaks Of Ephedrinementioning

confidence: 95%

Rapid on-site detection of ephedrine and its analogues used as adulterants in slimming dietary supplements by TLC-SERS

Cao

Lou

et al. 2014

Anal Bioanal Chem

View full text Add to dashboard Cite

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.

show abstract

“…Then, their peak intensity was used to calculate the relative standard deviation (RSD) value to Table S1). The precision of SERS is not as good as LC-MS or GC-MS [33].…”

Section: Analysis Of the Common And Characteristic Peaks Of Ephedrinementioning

confidence: 95%

Rapid on-site detection of ephedrine and its analogues used as adulterants in slimming dietary supplements by TLC-SERS

Cao

Lou

et al. 2014

Anal Bioanal Chem

View full text Add to dashboard Cite

show abstract

“…Based on studies by other researchers, the pentafluorophenylpropyl stationary phase is also recommended. 34,35,37 The HILIC is a promising and almost definite choice for separation of polar basic compounds that show separation problems under reverse based phases. The declaration on HILIC separation was based on testing basic alkyl-N hallucinogenic compounds on a fused core silica column.…”

Section: Discussionmentioning

confidence: 99%

“…The absence of publications on muscimol and psilocin, and the limited number of articles on simultaneous study of hallucinogens, might be an indication that the reverse phase alkyl columns are not the best in separating polar basic compounds as represented by the hallucinogenic alkaloids, a situation concurred by other researchers. 23,34,35 Almost all hallucinogens are alkaloids and contain an aromaticalkyl-N moiety that is basic at the N atom, except salvinorin A and tetrahydrocannabinol. The pentafluorophenylpropyl (PFP) stationary phase has been used successfully in separating some phenethylamine alkaloids.…”

Section: Introductionmentioning

confidence: 99%

“…[35][36][37] It has also been used on a combined mixture of eight tryptamine and phenethylamine derivatives in A. rigidula and its dietary extracts with only two analytes co-eluting. 34 When a C 18 column was used, five of the eight analytes could not be baseline separated. PFP is itself a reverse phase approach and has shown great separating ability for basic Nbased compounds.…”

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Comparative study of different column types for the separation of polar basic hallucinogenic alkaloids

Ncube¹,

Poliwoda²,

Cukrowska³

et al. 2016

S.Afr.j.chem.

View full text Add to dashboard Cite

The number of hallucinogenic compounds that have been separated simultaneously by liquid chromatography is limited. This research aimed to identify a column(s) that can allow for separation of several hallucinogens. The extent of separation of seven polar hallucinogenic tryptamine and phenethylamine derived alkaloids containing a basic N atom that becomes protonated at low pH values were investigated on five reverse-based columns and one hydrophilic interaction liquid chromatography (HILIC) column. An RP-phenyl and a negatively charged fused core HILIC were identified and recommended as effective columns in this regard. This research is the first to introduce a HILIC column in separation of hallucinogenic alkaloids and to simultaneously study the separation of the two principal psychoactive agents, muscimol and psilocin. The results of this study showed that better separation in HILIC columns can be achieved if an aprotic diluent of relatively lower polarity is used to introduce analytes into a mobile phase of higher polarity. Tetrahydrofuran was recommended where acetonitrile is used as the organic component of the mobile phase.

show abstract

“…[20] Neither BMPEA nor DMPPA have been detected in extracts of Acacia rigidula. [21] Similarly, multiple stimulants were discovered in a supplement called Dexaprine. Dexaprine contained the ephedrine analogues methylsynephrine (4-[1-hydroxy-2-(methylamino)propyl]phenol, 4-HMP, oxyephedrine, or oxilofrine (11)), synephrine (14), deterenol (14) and other amphetamine analogues.…”

mentioning

confidence: 99%

History full circle: ‘Novel’ sympathomimetics in supplements

Rasmussen

Keizers

2015

Drug Testing and Analysis

View full text Add to dashboard Cite

Since the banning of ephedrine in over-the-counter nutritional supplements a decade ago, a plethora of untested and/or unsafe sympathomimetic stimulants have taken its place. This paper argues that these 'novel' stimulants in supplements recapitulate the work of synthetic chemists at commercial pharmaceutical firms during the 1930s and 1940s, all seeking substitutes for recently successful products based on ephedrine and amphetamine.

show abstract

Determination of selected biogenic amines in Acacia rigidula plant materials and dietary supplements using LC–MS/MS methods

Cited by 58 publications

References 22 publications

Rapid on-site detection of ephedrine and its analogues used as adulterants in slimming dietary supplements by TLC-SERS

Rapid on-site detection of ephedrine and its analogues used as adulterants in slimming dietary supplements by TLC-SERS

Comparative study of different column types for the separation of polar basic hallucinogenic alkaloids

History full circle: ‘Novel’ sympathomimetics in supplements

Contact Info

Product

Resources

About