HPLC-UV-QDa analysis of Citrus aurantium-labelled pre-workout supplements suggest only a minority contain the plant extract

Koh, Andy Hsien Wei; Chess-Williams, Russ; Lohning, Anna

doi:10.1016/j.jpba.2020.113746

Cited by 10 publications

(12 citation statements)

References 28 publications

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“…Some discrepancies were observed between the quantity of total synephrine found in samples tested in this study and that from samples from the same batch tested in our previous non‐chiral analysis 7 . Five supplements in this study had higher amounts of total synephrine, four supplements had lower amounts of synephrine, and three supplements were the same as the previous analysis.…”

Section: Resultscontrasting

confidence: 82%

“…15 Indeed, we have previously reported that trace amine content in a sample of Citrus aurantium-listing pre-workout supplements was unlikely to be of plant origin based on the relative ratio of synephrine to other trace amines (p-octopamine and p-tyramine) normally found in Citrus aurantium. 7 Non-plant-based sources of synephrine could be further identified by determining the relative ratio of synephrine enantiomers, which can form the basis of a screen for authenticity in pre-workout supplements.…”

Section: Introductionmentioning

confidence: 99%

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Racemic synephrine found in Citrus aurantium‐listing pre‐workout supplements suggests a non‐plant‐based origin

Koh

Chess-Williams

Lohning

2021

Drug Testing and Analysis

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Multi‐ingredient pre‐workout supplements (MIPS) contain Citrus aurantium as a source of bioactive amines such as p‐synephrine, but concerns regarding the authenticity of ingredients in some supplements as well as adverse effects from consumption have been raised. R‐(−)‐Synephrine is the predominant enantiomer in Citrus aurantium extracts while synthetic preparations are often racemic. The aims of this study were to develop a screening method to determine the ratio of synephrine enantiomers in pre‐workout supplements listing Citrus aurantium and to assess the ingredient authenticity by directly comparing their ratios to that found in Citrus aurantium standardised reference materials (SRMs). Quantification of enantiomers in the supplements and SRMs was achieved using a validated, high‐performance liquid chromatography‐single quadrupole mass spectrometry (HPLC‐UV‐QDa) direct enantioseparation method with a cellobiohydrolase (CBH) column (100 × 4.0 mm, 5 μM) and UV detection at 225 nm. Citrus aurantium SRMs were found to have an average enantiomeric ratio of 94:6 (R:S) with total synephrine ranging from 5.7 to 90.2 mg/g. Within the pilot sample of pre‐workout supplements tested, only 42% (5/12) had enantiomeric ratios consistent with the SRMs with total synephrine ranging from 0.03 to 91.2 mg/g. For the remaining supplements, four had racemic ratios of synephrine (0.14 to 5.4 mg/g), two lacked any detectable levels of synephrine, and one had solely the S‐(+)‐enantiomer (0.15 mg/g). These results bring the authenticity of labelling of some pre‐workout supplements into question and highlight the need for more stringent labelling regulations and testing for dietary supplements.

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Section: Resultscontrasting

confidence: 82%

Section: Introductionmentioning

confidence: 99%

Racemic synephrine found in Citrus aurantium‐listing pre‐workout supplements suggests a non‐plant‐based origin

Koh

Chess-Williams

Lohning

2021

Drug Testing and Analysis

Self Cite

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“…This difference occurs because the d-or [S-(+)]-form provides little or no binding to adrenergic receptors in contrast to the lform [14]. This is important because a recent report suggests that most dietary supplements containing p-synephrine or Citrus aurantium do not contain the plant extract [15]. Therefore, the efficacy of commercially available supplements may be reduced when compared to natural products or plants' extracts for the same amount of p-synephrine.…”

Section: Chemical Structure Of P-synephrinementioning

confidence: 99%

“…Nevertheless, it is important to inform potential users of thermogenics and weight-loss products that other harmful stimulants may be included in commercially available dietary supplements, even when there is no information of the inclusion of these potentially dangerous substances on the label. The authenticity/quality assurance of dietary supplements containing p-synephrine [15], especially in those with a multi-ingredient formula, is key to avoiding potential side effects. The use of dietary supplements with pure p-synephrine is recommended to obtain its benefits on fat oxidation while reducing the likelihood of harmful effects due to the inclusion of other stimulants.…”

Section: Adverse Side Effects With Acute and Chronic Ingestion Of P-synephrinementioning

confidence: 99%

Effects of p-Synephrine during Exercise: A Brief Narrative Review

et al. 2021

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The p-synephrine is the principal phytochemical found in bitter orange (Citrus aurantium). This substance is widely included in dietary supplements for weight loss/body fat reduction due to its potential benefits of increasing fat oxidation. For years, p-synephrine-containing dietary supplements have been marketed without proper knowledge of their true effectiveness to enhance fat utilization, especially when combined with exercise. However, the effects of p-synephrine on fat oxidation during exercise have been investigated in the last few years. The aim of the current discussion is to summarize the evidence on the effects of p-synephrine intake on fat oxidation and performance during exercise. Previous investigations have demonstrated that the acute intake of p-synephrine does not modify running sprint performance, jumping capacity, or aerobic capacity. However, the acute intake of p-synephrine, in a dose of 2–3 mg/kg of body mass, has been effective to enhance the rate of fat oxidation during incremental and continuous exercise. This effect has been observed in a range of exercise workloads between 30% and 80% of peak oxygen uptake (VO2peak). The p-synephrine has the ability to increase the maximal rate of fat oxidation during exercise of increasing intensity without affecting the workload at which maximal fat oxidation is obtained (Fatmax). The effect of p-synephrine on fat oxidation is normally accompanied by a concomitant reduction of carbohydrate utilization during exercise, without modifying the energy expended during exercise. The shifting in substrate oxidation is obtained without any effect on heart rate during exercise and the prevalence of adverse effects is negligible. Thus, the acute use of p-synephrine, or p-synephrine-containing products, might offer some benefits for those individuals seeking higher fat utilization during exercise at low to moderate intensities. However, more research is still necessary to determine if the effect of p-synephrine on fat oxidation during exercise is maintained with chronic ingestion, in order to ascertain the utility of this substance in conjunction with exercise programs to produce an effective body fat/weight loss reduction.

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“…Establishment of the UHPLC-QDa-selected ion monitoring method In order to improve the detection sensitivity, a SIM method was developed that could achieve selective monitoring and intuitive exhibition of the targeted compounds [27]. As a modular single quadrupole MS detector, QDa provided a rapid confirmatory advantage over conventional HPLC-UV methods and exhibited comparable performance to MS/MS in qualitative and quantitative analysis of herbal medicine [28,29]. In addition, taking practicability and accessibility into consideration, QDa was more suitable for routine analysis of TCM.…”

Section: 22mentioning

confidence: 99%

A strategy for practical authentication of medicinal plants in traditional Chinese medicine prescription, paeony root in ShaoYao‐GanCao decoction as a case study

Cheng

Yao

et al. 2021

J of Separation Science

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Authentication of Chinese medicine materials in prescriptions is extremely difficult due to the complicated chemical matrix. A strategy integrating in-depth profiling, chemical marker selection, and selected detection was established and exemplarily applied to authenticate paeony root in ShaoYao-GanCao decoction. First, an ultra-performance liquid chromatography/linear trap quadrupole-Orbitrap method was developed to probe the chemical compositions of the decoction. Second, 20 batches of decoctions prepared from white paeony root and red paeony root were compared by a metabolomics method, and multistep chemometrics analysis distinguished the chemical markers. Third, an ultraperformance liquid chromatography/QDa-selected ion monitoring method was developed to authenticate the paeony root in decoctions. As a result, 161 compounds were characterized, including 84 triterpene saponins, 42 flavonoids, and 10 monoterpenes. Four chemical markers and paeoniflorin were successfully screened out as chemical markers for white paeony root. The selected ion monitoring method easily differentiated authentic decoction (prepared from white paeony root) from fraud decoction (prepared from red paeony root) by monitoring the above five chemical markers. In conclusion, the strategy was proved effective in authentication of paeony root in ShaoYao-GanCao decoction, and it can also be applied to authenticate other Chinese medicine materials in prescriptions, which will greatly avail the quality enhancement of prescriptions.

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HPLC-UV-QDa analysis of Citrus aurantium-labelled pre-workout supplements suggest only a minority contain the plant extract

Cited by 10 publications

References 28 publications

Racemic synephrine found in Citrus aurantium‐listing pre‐workout supplements suggests a non‐plant‐based origin

Racemic synephrine found in Citrus aurantium‐listing pre‐workout supplements suggests a non‐plant‐based origin

Effects of p-Synephrine during Exercise: A Brief Narrative Review

A strategy for practical authentication of medicinal plants in traditional Chinese medicine prescription, paeony root in ShaoYao‐GanCao decoction as a case study

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