Simultaneous determination of eight alkaloids and oleandrin in herbal cosmetics by dispersive solid‐phase extraction coupled with ultra high performance liquid chromatography and tandem mass spectrometry

Abstract

We utilized ultra-high performance liquid chromatography with tandem mass spectrometry and dispersive solid-phase extraction to develop a new method for the detection of nine analytes (scopolamine, cephaeline, strychnine, hyoscyamine, brucine, hydrastine, ajmalicine, colchicine, and oleandrin) in herbal cosmetics. Acetonitrile/water and 2-propylaminoethylamine were used to disperse and purify during the dispersive solid-phase extraction step. The analytes were separated by a Waters UPLC HSS T3 column and detected through electrospray ionization source in the positive mode with multi-reaction monitoring conditions. Under the optimal conditions, the calibration curves were linear in the range of 0.2-100.0 μg/L with the correlation coefficients higher than 0.995. The method limit of quantitation (S/N = 10) were 5.0 μg/kg for oleandrin and 1.0 μg/kg for the other eight alkaloids. The mean recoveries at three spiked concentration levels of 1.0-10.0 μg/kg were in the range of 86.9-116.5% with the intra-day relative standard deviations (n = 6) ranging from 2.4 to 8.8%, and inter-day relative standard deviations ranging from 2.7 to 5.7%. This method is accurate, simple and rapid, and has been applied to the quality supervision of herbal cosmetics in Guangzhou.

Development of a UHPLC–MS/MS method for the quantitation of bioactive compounds in Phyllanthus species and its herbal formulations

“…Compared with the HPLC and HPTLC methods, the UHPLC-ESI-MS/MS method in multiple reaction monitoring (MRM) acquisition mode is more effective in rapidly quantifying trace compounds due to its rapid separation power, low detection limit, better accuracy, high specificity, and resolution [12,[35][36][37][38][39].…”

Oleandrin: A Systematic Review of its Natural Sources, Structural Properties, Detection Methods, Pharmacokinetics and Toxicology

“…Owing to the sensitivity and specificity of LC-MS technology, attempts were made to use this method in as early as 1993 to confirm oleandrin in decayed human tissues ( Rule et al, 1993 ). Recent studies have indicated that trace-level oleandrin can be rapidly and accurately analyzed in various complex biological samples, both qualitatively and quantitatively using LC-MS/MS ( Song et al, 2017 ; Xun et al, 2017 ; Ying et al, 2017 ; Botelho et al, 2018 ; Zhai et al, 2018 ; Gosetti et al, 2019 ; Oishi et al, 2019 ; Ceci et al, 2020 ). As such, LC-MS/MS analysis has evolved into the best choice for pharmacokinetic and experimental toxicological studies of oleandrin ( Tor et al, 2005 ).…”

Interpol review of controlled substances 2016–2019

“…Abused Substances Illegally Added to Licit Pharmaceuticals, Herbal Medications, Health Supplements, and Foodstuffs (Notes: A) Specific, named compounds are compiled in their individual categories above; B) There are many dozens/hundreds of (highly repetitive) articles pertaining to adulteration of Chinese foods, food seasonings, health care supplements, sexual enhancement aids, Chinese Traditional Medicines, etc. ; only a subset of these are included below) : 2016 Amphetamine and derivatives in natural weight loss pills and dietary supplements with a modified QuEChERS extraction procedure by followed by CE-MS/MS analysis [ 1319 ]; review to discuss the current literature on food-derived opioid peptides focusing on their production, methods of detection, isolation and purification [ 1320 ]; H1-NMR detection, identification and quantification of adulterants (active pharmaceutical ingredients) in 160 herbal food supplements marketed for weight loss [ 1321 ]; development and validation of UPLC and LC-MS/MS methods for the simultaneous determination of anti-obesity drugs in foods and dietary supplements [ 1322 ]; analysis of trace amounts of adulterants found in powders/supplements RAMAN coupled to direct analyte-probed nanoextraction-nanospray IMS [ 1323 ]; LC-ESI-MS/MS method for the simultaneous detection of common synthetic drugs as adulterants in natural and herbal slimming products [ 1324 ]; LC-MS/MS analysis of 40 wt loss compounds adulterated in health supplements including bisacodyl, phenolphthalein, and sibutramine and its metabolites [ 1325 ]; banned and discouraged-use ingredients found in weight loss supplements [ 1326 ]; detection of adulterants in botanical dietary supplements by TLC combined with SERS [ 1327 ]; identification of chemical compounds in Mahuang-Fuzi-Xixin Decoction by HPLC-QQQ/MS/MS and HPLC-QQQ/MS/MS [ 1328 ]; comparison of HPLC-UV and CE analysis of weight loss supplements [ 1329 ]; HPLC method for determination of the ingredients in cough syrup [ 1330 ]; desktop ion trap MS coupled with PSI, ESI and slug-flow microextraction for direct analysis of illegal substances in various types of cosmetic and foodstuff samples [ 1331 ]; review of adulteration of dietary supplements by the illegal addition of synthetic drugs [ 1332 ]; 2017 Four experimental stimulants identified by UHPLC-MS in sports and weight loss supplements: 2-amino-6-methylheptane (octodrine), 1,4-dimethylamylamine (1,4-DMAA), 1,3-dimethylamylamine (1,3-DMAA) and 1,3-dimethylbutylamine (1,3-DMBA) [ 1333 ]; biosensor-based two-phase pharmacological profiling for discovery, monitor and control of natural products [ 1334 ]; simultaneous determination of eight alkaloids and oleandrin in herbal cosmetics by dispersive SPE coupled with UHPLC-MS/MS [ 1335 ]; validated UHPLC-LTQ-Orbitrap HRMS method for identification, confirmation and quantitation of illegal adulterated weight-loss drugs in plant dietary supplements [ 1336 ]; UPLC-PDA and an UPLC-MS method were developed to analyze 92 slimming aids (confiscated by customs) [ ...…”