Application of liquid chromatography‐high resolution mass spectrometry and liquid chromatography‐tandem mass spectrometry methods to 45 weight loss compounds in health functional food, food, and illegal drug

Abstract

In order to effectively and quickly monitor such illegal food and drugs, simultaneous screening and quantitative analysis for multiple compounds are needed. In this study, we established a method of identifying fragmentation ions of 45 compounds for weight loss using liquid chromatography and high‐resolution mass spectrometry and developed a quantitation method through liquid chromatography and tandem mass spectrometry. Note that, 656 samples selected as health functional food, food, and illegal drug were applied. The detection rate of banned weight loss compounds in health functional food, food, and illegal drug was showed as 19.2, 27.3, 40.7%, respectively. Among them, sibutramine, sennoside A and B, ephedrine were most frequently detected in 237 samples that contained weight loss compounds. The detection range about sibutramine was 0.03–159.3 mg/g, sennoside was 0.1–97.6 mg/g, and ephedrine was 0.1–587.7 mg/g in the detected 237 samples. In addition, the unknown compounds not included in our simultaneous analysis method in some samples were identified as furosemide and chlorpheniramine. High selectivity of high resolution mass spectrometry combined with these fragmentation pathways and tandem mass spectrometry methods can be successfully applied to screening and identifying 45 weight loss compounds for continuous blocking and supervision of illegally distributed health functional food, food, and illegal drug.

Establishment of high‐performance liquid chromatography‐photodiode array method for 43 weight loss agents and effect of basic environment on bisacodyl degradation

“…The LC-Q-Orbitrap/MS method proposed in this study and the HPLC-PDA method in combination could be used to discriminate isomers that cannot be identified using only HPLC-PDA. 19 In addition, we presented not only the PDA spectra for the 43 components analyzed in this study but also the MS 2 spectra with proposed fragment ion structures obtained using LC-Q-Orbitrap/MS used to identify each peak produced by bisacodyl degradation. Therefore, our developed HPLC-PDA method could be useful for detecting 43 weight loss components, and our MS 2 data on the degradation products of bisacodyl could be used as a valuable resource for researchers developing analytical methods targeting bisacodyl.…”

“…Validation data for the developed HPLC‐PDA method demonstrate that it is sufficiently reliable to quickly identify and quantify unauthorized pharmaceutical active ingredients in illegal products. The LC‐Q‐Orbitrap/MS method proposed in this study and the HPLC‐PDA method in combination could be used to discriminate isomers that cannot be identified using only HPLC‐PDA. 19 In addition, we presented not only the PDA spectra for the 43 components analyzed in this study but also the MS 2 spectra with proposed fragment ion structures obtained using LC‐Q‐Orbitrap/MS used to identify each peak produced by bisacodyl degradation.…”

Adulteration of Brain Health (Cognitive, Mood, and Sleep Enhancement) Food Supplements by the Addition of Pharmaceutical Drugs: A Comprehensive Review of Analytical Approaches and Trends

“…However, the analyzed supplements purported activities other than brain-related functions, such as weight loss. Lee et al [ 79 ] proposed the use of LC-Q-Orbitrap-MS to screen the presence of drugs in weight-loss supplements, followed by subsequent analysis of the identified adulterated products by LC-MS/MS, which was validated to allow the quantification of 45 compounds. In addition to banned anorexics, laxatives, and related compounds, weight-loss supplements have been found to contain substances with diverse pharmacological activities, including antidepressants and stimulants [ 11 ].…”

“…As far as the literature consulted, data on the consumption prevalence of supplements to improve mood or sleep are still scarce or non-existent. However, the U.S. National Poll on Healthy Aging (NPHA) survey, targeting a community of older adults that included 1065 community-dwelling adults (aged [65][66][67][68][69][70][71][72][73][74][75][76][77][78][79][80], showed that about 35% suffered from sleep-specific difficulties and resorted to the use of sleep improvement products, namely 21.9% use over the counter sleep products, 12.5% consume herbal-containing products, and 8.3% use prescription medication [55]. In addition, it was recently reported that in the U.S., the use of melatonin, a key regulator of the circadian rhythm purportedly involved in sleep disorders and frequently added as an ingredient in PFS, has increased from 0.4% in 1999-2000 to 2.1% in 2017-2018 [56].…”

Targeted quantitative analysis of monoterpenoid indole alkaloids in Alstonia scholaris by ultra‐high‐performance liquid chromatography coupled with quadrupole time of flight mass spectrometry

“…Although low or unit resolution triple quadrupole mass spectrometer in selected reaction monitoring or multiple reaction monitoring mode is considered the “gold standard” in the quantitative analysis of small molecules [15, 16], limitations, such as restricted detection number of analytes at the same time and confined selectivity caused by limited resolution, still exist [15, 17]. In recent years, UHPLC coupled with high‐resolution MS (HRMS) has triggered new techniques for the quick qualitative and targeted quantitative analysis [18] of phytochemicals [11, 19, 20] and drugs [21, 22]. The limitations in triple quadrupole mass spectrometer detection caused by a unit or low resolution can be compensated by the application of HRMS instruments [17].…”