Current trends in the analysis and quality control of food supplements based on plant extracts.

Food (dietary) supplements include a wide range of products that are designed to be taken because of their added nutrients and presumed health benefits. Global food supplement sales are experiencing rapid growth and supplements that based on botanicals are among the most popular. The meteoric rise in sales coupled with the general lack of a commitment to pass effective regulation make this market more vulnerable to dishonest producers, increase the likelihood that supplements containing adulterants are sold on the market, and a greater prevalence of safety and quality issues (contamination by pesticides and mycotoxins). In this paper, we present an overview of various sample preparation and analytical techniques that can be used for the determination of bioactive substances in food supplements based on plant extracts and for making purity assessments of plant extracts in these preparations. The analysis looks at data collected from 2012 to 2017. The work is divided according to the different approaches taken when analysing food supplements and groups of bioactive substances found in plant extracts (purity assessments and the determination of bioactive substances).

[1]  I. Khan,et al.  Ultra-HPLC method for quality and adulterant assessment of steviol glycosides sweeteners – Stevia rebaudiana and stevia products , 2015, Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment.

[2]  Roberto Romero-González,et al.  Multi-class methodology to determine pesticides and mycotoxins in green tea and royal jelly supplements by liquid chromatography coupled to Orbitrap high resolution mass spectrometry. , 2016, Food chemistry.

[3]  A. G. Frenich,et al.  Multi-pesticide residue analysis in nutraceuticals from grape seed extracts by gas chromatography coupled to triple quadrupole mass spectrometry , 2015 .

[4]  Ji Hye Jeong,et al.  Determination of Miroestrol and Isomiroestrol From Pueraria mirifica (White Kwao Krua) in Dietary Supplements by LC-MS-MS and LC-Q-Orbitrap/MS. , 2017, Journal of chromatographic science.

[5]  Véronique Gilard,et al.  Proton NMR for detection, identification and quantification of adulterants in 160 herbal food supplements marketed for weight loss. , 2016, Journal of pharmaceutical and biomedical analysis.

[6]  E. Castrignanò,et al.  Liquid chromatography-high resolution mass spectrometry (LC-HRMS) determination of stimulants, anorectic drugs and phosphodiesterase 5 inhibitors (PDE5I) in food supplements. , 2015, Journal of pharmaceutical and biomedical analysis.

[7]  L. Ye,et al.  Dispersive Micro Solid-Phase Extraction with Graphene Oxide for the Determination of Phenolic Compounds in Dietary Supplements by Ultra High Performance Liquid Chromatography Coupled with Quadrupole Time-of-Flight Tandem Mass Spectrometry , 2015, Food Analytical Methods.

[8]  I. Khan,et al.  Simultaneous determination of sesquiterpenes and pyrrolizidine alkaloids from the rhizomes of Petasites hybridus (L.) G.M. et Sch. and dietary supplements using UPLC-UV and HPLC-TOF-MS methods. , 2012, Journal of pharmaceutical and biomedical analysis.

[9]  P. Solich,et al.  A Fast HPLC Method for Determination of Vitamin E Acetate in Dietary Supplements Using Monolithic Column , 2013, Food Analytical Methods.

[10]  Bharathi Avula,et al.  Concurrent supercritical fluid chromatographic analysis of terpene lactones and ginkgolic acids in Ginkgo biloba extracts and dietary supplements , 2016, Analytical and Bioanalytical Chemistry.

[11]  Katerina Mastovska,et al.  Mycotoxins in Plant-Based Dietary Supplements: Hidden Health Risk for Consumers. , 2015, Journal of agricultural and food chemistry.

[12]  B. Venhuis,et al.  Towards a decade of detecting new analogues of sildenafil, tadalafil and vardenafil in food supplements: a history, analytical aspects and health risks. , 2012, Journal of pharmaceutical and biomedical analysis.

[13]  Roberto Romero-González,et al.  Multifamily determination of pesticide residues in soya-based nutraceutical products by GC/MS-MS. , 2015, Food chemistry.

[14]  N. Brosse,et al.  UPLC method for the determination of vitamin E homologues and derivatives in vegetable oils, margarines and supplement capsules using pentafluorophenyl column. , 2014, Talanta.

[15]  I. Vovk,et al.  Determination of lutein by high-performance thin-layer chromatography using densitometry and screening of major dietary carotenoids in food supplements. , 2012, Journal of chromatography. A.

[16]  E. Sieniawska,et al.  LC-QTOF-MS Analysis and Activity Profiles of Popular Antioxidant Dietary Supplements in Terms of Quality Control , 2017, Oxidative medicine and cellular longevity.

[17]  A. Marseglia,et al.  A simple GC-MS method for the screening of betulinic, corosolic, maslinic, oleanolic and ursolic acid contents in commercial botanicals used as food supplement ingredients. , 2013, Food chemistry.

[18]  Qingxia Zhu,et al.  Rapid on-site TLC–SERS detection of four antidiabetes drugs used as adulterants in botanical dietary supplements , 2014, Analytical and Bioanalytical Chemistry.

[19]  H. Lieberman,et al.  Analysis of 1,3 dimethylamylamine concentrations in Geraniaceae, geranium oil and dietary supplements. , 2014, Drug testing and analysis.

[20]  A. Calderón,et al.  Liquid chromatography/mass spectrometry based fingerprinting analysis and mass profiling of Euterpe oleracea (açaí) dietary supplement raw materials. , 2012, Food chemistry.

[21]  Li-Hui Yin,et al.  Detection of illegally added drugs in dietary supplements by near-infrared spectral imaging , 2014 .

[22]  E. Deconinck,et al.  Detection of regulated herbs and plants in plant food supplements and traditional medicines using infrared spectroscopy , 2017, Journal of pharmaceutical and biomedical analysis.

[23]  L. Yu,et al.  Chemical profiling of glucosinolates in cruciferous vegetables-based dietary supplements using ultra-high performance liquid chromatography coupled to tandem high resolution mass spectrometry , 2017 .

[24]  P. Solich,et al.  A UHPLC method for the rapid separation and quantification of phytosterols using tandem UV/Charged aerosol detection – A comparison of both detection techniques , 2017, Journal of pharmaceutical and biomedical analysis.

[25]  S. Zeng,et al.  Application of a high resolution benchtop quadrupole-Orbitrap mass spectrometry for the rapid screening, confirmation and quantification of illegal adulterated phosphodiesterase-5 inhibitors in herbal medicines and dietary supplements. , 2014, Journal of chromatography. A.

[26]  Sung-Kwan Park,et al.  Simultaneous analysis of 35 specific antihypertensive adulterants in dietary supplements using LC/MS/MS. , 2017, Biomedical chromatography : BMC.

[27]  P. Solich,et al.  A new approach to the rapid separation of isomeric compounds in a Silybum marianum extract using UHPLC core‐shell column with F5 stationary phase , 2017, Journal of pharmaceutical and biomedical analysis.

[28]  P. Solich,et al.  A study of retention characteristics and quality control of nutraceuticals containing resveratrol and polydatin using fused-core column chromatography. , 2016, Journal of pharmaceutical and biomedical analysis.

[29]  Shiuh-Jen Jiang,et al.  Combined use of HPLC-ICP-MS and microwave-assisted extraction for the determination of cobalt compounds in nutritive supplements. , 2014, Food Chemistry.

[30]  M. Ganzera,et al.  Supercritical fluid chromatography for the separation of isoflavones. , 2015, Journal of pharmaceutical and biomedical analysis.

[31]  Z. Ali,et al.  Chemical fingerprint analysis and quantitative determination of steroidal compounds from Dioscorea villosa, Dioscorea species and dietary supplements using UHPLC-ELSD. , 2014, Biomedical chromatography : BMC.

[32]  Bashir Ahmad,et al.  Natural occurrence of mycotoxins in medicinal plants: a review. , 2014, Fungal genetics and biology : FG & B.

[33]  Bin Guo,et al.  Wide-Scope Screening of Illegal Adulterants in Dietary and Herbal Supplements via Rapid Polarity-Switching and Multistage Accurate Mass Confirmation Using an LC-IT/TOF Hybrid Instrument. , 2015, Journal of agricultural and food chemistry.

[34]  T. Begley,et al.  Determination of multiple mycotoxins in dietary supplements containing green coffee bean extracts using ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). , 2013, Journal of agricultural and food chemistry.

[35]  P. Solich,et al.  A Fast Determination of Chlorophylls in Barley Grass Juice Powder Using HPLC Fused-Core Column Technology and HPTLC , 2014, Food Analytical Methods.

[36]  M. Plotan,et al.  Estrogenic endocrine disruptors present in sports supplements. A risk assessment for human health. , 2014, Food chemistry.

[37]  Joana S. Amaral,et al.  Analysis of pharmaceutical adulterants in plant food supplements by UHPLC‐MS/MS , 2017, European journal of pharmaceutical sciences : official journal of the European Federation for Pharmaceutical Sciences.

[38]  Lukáš Václavík,et al.  Targeted analysis of multiple pharmaceuticals, plant toxins and other secondary metabolites in herbal dietary supplements by ultra-high performance liquid chromatography-quadrupole-orbital ion trap mass spectrometry. , 2014, Analytica chimica acta.

[39]  P. Jones,et al.  Development of an improved reverse-phase high-performance liquid chromatography method for the simultaneous analyses of trans-/cis-resveratrol, quercetin, and emodin in commercial resveratrol supplements. , 2014, Journal of agricultural and food chemistry.

[40]  D. Šatínský,et al.  A New Gas Chromatography Method for Quality Control of Methylsulfonylmethane Content in Multicomponent Dietary Supplements , 2014, Food Analytical Methods.

[41]  R. Fernández-Torres,et al.  New developments in microextraction techniques in bioanalysis. A review. , 2016, Analytica chimica acta.

[42]  P. Solich,et al.  A UHPLC method for the rapid separation and quantification of anthocyanins in acai berry and dry blueberry extracts , 2017, Journal of Pharmaceutical and Biomedical Analysis.

[43]  M. Dell’Agli,et al.  Development and validation of HPLC method to measure active amines in plant food supplements containing Citrus aurantium L , 2014 .

[44]  A. G. Frenich,et al.  Multi-class determination of pesticides and mycotoxins in isoflavones supplements obtained from soy by liquid chromatography coupled to Orbitrap high resolution mass spectrometry , 2016 .

[45]  M. Shamsipur,et al.  Recent advances in liquid-phase microextraction techniques for the analysis of environmental pollutants , 2017 .

[46]  A. M. García-Campaña,et al.  High-Throughput Methodology for the Determination of Carbamates in Food Supplements by UHPLC–MS/MS , 2016, Chromatographia.

[47]  E. Szłyk,et al.  Determination of toxic metals by ICP-MS in Asiatic and European medicinal plants and dietary supplements. , 2015, Journal of trace elements in medicine and biology : organ of the Society for Minerals and Trace Elements.

[48]  Shiuh-Jen Jiang,et al.  Determination of selenium compounds in food supplements using reversed-phase liquid chromatography–inductively coupled plasma mass spectrometry , 2013 .

[49]  A. Romani,et al.  Polyphenols and secoiridoids in raw material (Olea europaea L. leaves) and commercial food supplements , 2017, European Food Research and Technology.

[50]  J. López-Hernández,et al.  Comparison of methods for analysis of resveratrol in dietary vegetable supplements. , 2017, Food chemistry.

[51]  Łukasz Marcinkowski,et al.  Green aspects, developments and perspectives of liquid phase microextraction techniques. , 2014, Talanta.

[52]  A. G. Frenich,et al.  Quality control evaluation of nutraceutical products from Ginkgo biloba using liquid chromatography coupled to high resolution mass spectrometry. , 2016, Journal of pharmaceutical and biomedical analysis.

[53]  D. Lachenmeier,et al.  NMR evaluation of total statin content and HMG-CoA reductase inhibition in red yeast rice (Monascus spp.) food supplements , 2012, Chinese Medicine.

[54]  P. Solich,et al.  A New and Fast HPLC Method for Determination of Rutin, Troxerutin, Diosmin and Hesperidin in Food Supplements Using Fused-Core Column Technology , 2013, Food Analytical Methods.

[55]  S. Magiera,et al.  UHPLC-UV method for the determination of flavonoids in dietary supplements and for evaluation of their antioxidant activities. , 2015, Journal of pharmaceutical and biomedical analysis.

[56]  M. Hengel,et al.  Multiresidue pesticide analysis of botanical dietary supplements using salt-out acetonitrile extraction, solid-phase extraction cleanup column, and gas chromatography-triple quadrupole mass spectrometry. , 2013, Analytical chemistry.

[57]  Wei Liu,et al.  Application of ultra-high performance supercritical fluid chromatography for the determination of carotenoids in dietary supplements. , 2015, Journal of chromatography. A.

[58]  K. Héberger,et al.  Quantitative determination of coenzyme Q10 from dietary supplements by FT-NIR spectroscopy and statistical analysis , 2015, Analytical and Bioanalytical Chemistry.

[59]  P. Solich,et al.  A new method for rapid determination of indole-3-carbinol and its condensation products in nutraceuticals using core-shell column chromatography method. , 2016, Journal of pharmaceutical and biomedical analysis.

[60]  P. Plaza-Bolaños,et al.  Identification and quantification of phytochemicals in nutraceutical products from green tea by UHPLC-Orbitrap-MS. , 2015, Food chemistry.

[61]  A. M. Troncoso,et al.  Quality control and determination of melatonin in food supplements , 2016 .

[62]  Mihaela Badea,et al.  Quality control of plant food supplements. , 2011, Food & function.

[63]  M. Malet‐Martino,et al.  Detection, identification and quantification by 1H NMR of adulterants in 150 herbal dietary supplements marketed for improving sexual performance. , 2015, Journal of pharmaceutical and biomedical analysis.

[64]  L. Nováková,et al.  Development of matrix effect‐free MISPE‐UHPLC–MS/MS method for determination of lovastatin in Pu‐erh tea, oyster mushroom, and red yeast rice , 2017, Journal of pharmaceutical and biomedical analysis.

[65]  L. Sánchez-Hernández,et al.  Chiral analysis of aromatic amino acids in food supplements using subcritical fluid chromatography and Chirobiotic T2 column , 2016 .

[66]  A. G. Frenich,et al.  Determination of toxic substances, pesticides and mycotoxins, in ginkgo biloba nutraceutical products by liquid chromatography Orbitrap-mass spectrometry , 2015 .

[67]  J. Antignac,et al.  The application of reporter gene assays for the detection of endocrine disruptors in sport supplements. , 2011, Analytica chimica acta.

[68]  F. Longobardi,et al.  Food coloring agents and plant food supplements derived from Vitis vinifera: a new source of human exposure to ochratoxin A. , 2015, Journal of agricultural and food chemistry.

[69]  Roberto Romero-González,et al.  Application of QuEChERS based method for the determination of pesticides in nutraceutical products (Camellia sinensis) by liquid chromatography coupled to triple quadrupole tandem mass spectrometry. , 2015, Food chemistry.

[70]  M. Plotan,et al.  Validation and application of reporter gene assays for the determination of estrogenic and androgenic endocrine disruptor activity in sport supplements , 2012, Analytical and Bioanalytical Chemistry.

[71]  Ermias A. Haile,et al.  Quantification of plant sterols/stanols in foods and dietary supplements containing added phytosterols , 2015 .