Determination of synthetic drugs used to adulterate botanical dietary supplements using QTRAP LC-MS/MS

Y, Chen; Zhao, Lei; Lu, Feng; Yu, Yanlei; Chai, Yifeng; Wu, Yutian

doi:10.1080/02652030802641880

Cited by 63 publications

(26 citation statements)

References 17 publications

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“…For most adulterants, 1 % is always the smallest amount of adulterant with high and instant efficacy [40,41], therefore, the limit of detection (LOD) of 1 % is sufficient for detection of most cases of adulteration. In SERS detection, the LOD is determined by the lowest amount of a chemical in the laser spot that can generate a spectrum significantly distinct from the background [29].…”

Section: Analysis Of Simulated Positive Samplesmentioning

confidence: 99%

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

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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.

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Section: Analysis Of Simulated Positive Samplesmentioning

confidence: 99%

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

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“…In fact the Brazilian National Agency of Sanitary Vigilance (ANVISA) has reported cases of adulteration of athlete food and complements beverages. 14 The United State Pharmacopoeia does not indicate an official method for the quantification of sibutramine hydrochloride monohydrate, but a few methods have been described in the literature using high performance liquid chromatography with UV photometric 15 and mass spectrometric detection, 16,17 capillary electrophoresis with UV detetion, 7,18 UV absorption spectrophotometry 19 and infrared spectroscopy. 20 Voltammetric methods enable the sensitive and selective measurement of organic compounds based on their specific electrochemical behavior at the working electrode surface.…”

Section: Sibutramine N-(1-(1-(4-chlorophenyl)-cyclobutyl)-3-methylbumentioning

confidence: 99%

Voltammetric determination of sibutramine in beverages and in pharmaceutical formulations

Carvalho¹,

Silva²,

Cunha³

et al. 2012

Quím. Nova

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Recebido em 6/10/11; aceito em 30/11/11; publicado na web em 23/1/12 A simple and sensitive method has been proposed for the determination of sibutramine-HCl in energy drinks, green tea and pharmaceutical formulations using differential pulse voltammetry performed on a hanging mercury drop electrode. In the chosen experimental condition (Mcllvaine pH 4.0 buffer, 50 mV pulse amplitude and 40 mV s -1 scan velocity), sibutramine-HCl presented a reversible behavior and a peak maximum at -80 mV. Detection limit was 0.4 mg L -1 and the working linear range extended up to 33.3 mg L -1 (r = 0.99). Analysis of real and fortified samples enabled recoveries between 91 and 102%. The electroanalytical method was compared with a HPLC method which indicated it accuracy.

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“…These specific fragmentation peaks indicate that the parent peak of m/z 319.0 is phenolphthalein. 4,12 …”

Section: Resultsmentioning

confidence: 99%

Analysis of trace amounts of adulterants found in powders/supplements utilizing Raman spectroscopy coupled to direct analyte-probed nanoextraction-nanospray ionization-mass spectrometry

et al. 2016

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In the United States, all food products have to be regulated to inform the consumers of the ingredients contained within. Some ingredients are not included on the label and yet are still found in the products. Presented is a Raman imaging technique for rapid, nondestructive, and spatially relevant localization of adulterants in powders. Raman spectroscopy followed by direct analyte-probed nanoextraction coupled to nanospray ionization-mass spectrometry allows rapid determination of the presence of each adulterant, leading to positive identifications such as melamine. The location and identification of these trace particles can then be extracted using a nanomanipulator. The nanomanipulation technique uses a solvent filled capillary tip which can be positioned on the particle of interest. Direct mass spectrometric analysis via nanospray of the particulate of interest eliminates time consuming chromatographic techniques prior to mass spectrometry analysis. This coupled technique combines rapid Raman spectroscopy techniques with direct mass spectrometry to confirm the presence of an adulterant. This technique was applied to an FDA supplied test sample, in which sibutramine, phenolphthalein, and melamine were confirmed to be present.

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Determination of synthetic drugs used to adulterate botanical dietary supplements using QTRAP LC-MS/MS

Cited by 63 publications

References 17 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

Voltammetric determination of sibutramine in beverages and in pharmaceutical formulations

Analysis of trace amounts of adulterants found in powders/supplements utilizing Raman spectroscopy coupled to direct analyte-probed nanoextraction-nanospray ionization-mass spectrometry

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