Number of analyzed dietary supplements Number of dietary supplements that contain undeclared substances Undeclared substances Main results Methods for detection Country of origin Ref. 634 94 Теstosterone, 4-norendionon, 4-аdendion, 5-adendiol, nandrolone, boldenone, dehydroepiandrosterone (DHEA) 14.8% positive supplements showed anabolic steroid concentrations from 0.01 μ g/g up to 190 μ g/g GC-MS Germany [36 ] 75 7 DHEA, 19-noranrostenedione, ephedrine Seven products had hormones that were not listed on the labels, and two more products contained ephedrine and caffeine that were not clearly labeled GC-MS Switzerland [23 ] 103 3 Nandrolone, testosterone, 4-androstenediol, androstenediol, androstenedione, bolasterone, boldenone, clostebol, DHEA, dihydrotestosterone (DHT), drostanolone, fluoxymesterone, mesterolone,4-norandrostenediol, 5-androstenedione, 5-norandrostenediol, 19-noranrostenedione, metandienone, metenolone, methyltestosterone, norethandrolone, oxandrolone, oxymesterone, stanozol, oxymetholone, testosterone propionate, 5-norandrostenedione An amount of metandienone in three supplements in a range from 0.41 mg/g up to 17.30 mg/g was found GC-MS Switzerland [37 ] 12 11 Testosterone, 5-androstenediol, 4-androstene-3,17-dione, 5-androstene-3,17-diol, 19-androstene-3b, 17b-diol Supplements did not meet the labeling requirements. One supplement contained 10 mg of testosterone; another contained 77% more than the label stated; 11 of the 12 contained less than what was indicated HPLC, GC-MS USA [38 ] 64 8 Nandrolone decanoate, testosterone decanoate, 4-androstendion, ephedrine, DHEA Concentration range: 1–25 ng/g LC-MS/MS Italy [39 ] 19 15 Тestosterone, beta-boldenone, alfa-boldenone, beta-nortestosterone Concentrations between 0.01 mg/g and 2.5 mg/per capsule or tablet were found. Testosterone was in most samples (50%) LC-MS/MS Belgium [40 ] 16 9 1,3-Dimethylamylamine (DMAA) Concentration range: 3.1 mg/g-415 mg/g NMR Germany [28 ] 112 6 Dehydroepiandrosterone (DHEA) Concentration range:1-500 ng/g Androgen bioassay New Zealand [41 ] 19 2 Higenamine Concentrations 6.42 ng/mL and 18.93 ng/mg were found in two samples UHPLC-MS/MS Serbia [42 ] 24 5 Higenamine Dosages of up to UHPLC-MS/MS USA, Netherlands [43 ] 6 6 D6-Methyltestosterone, methasterone, prostanozol After positive doping samples, 6 dietary supplements were tested and all have undeclared substances GC-MS Germany [44 ] 10 2 Sibutramine More than 20 mg per tablet was found Ultra-high-performance liquid chromatography-high-resolution mass spectrometry (UHPLC-HRMS) Bulgaria [31 ] 20 14 Andarine, ostarine, ibutamoren, arimistane The amounts of these undeclared analytes ranged from 0.6 mg per capsule to 6.8 mg per capsule UHPLC UK [26 ] 188 29 Sibutramine Concentrations of detected sample range from 0.03 mg/g up to 132.40 mg/g LC-MS/MS South Korea [32 ] 123 24 Sibutramine Sibutramine contents in green coffee samples were 0.014–2 438 mg/kg; the highest content of sibutramine was found in one capsule sample (26 410 mg/kg) LC-ESI-MS/MS Croatia [33 ] 200 27 Synephrine, yohimbine, 5-hydroxytryptophan, DHEA The concentrations of detected samples ranged from 0.51 mg/g up to 226 mg/g LC-MS/MS South Korea [35 ] 13 13 DMAA Concentration range from 0.1 mg/g to 110 mg/g HPLC-MS USA [29 ] 8 7 Sibutramine, phenolphthalein, bumetanide, phenytoin Concentrations of sibutramine ranged from 6 mg up to 57 mg per capsule LC-MS Iran [34 ] 50 24 Sibutramine, rimonabant, desmethylsibutramine, didesmethylsibutramine, sildenafil Concentrations of sibutramine ranged from 0.1 mg up to 21 mg per capsule HPLC-DAD-MS/MS Netherlands [45 ] 52 11 Theobromine, theophylline, pseudoephedrine, caffeine, hydrochlorothiazide, yohimbinе Hydrochlorothiazide content found: 0.01 mg-0.37 mg UHPLC-DAD Saudi Arabia [48 ] 5 5 Sibutramine, 4-hydroxyamphetamine, caffeine, theophylline Sibutramine content found: 15 and 26 mg/g HRAM screening Italy [49 ] Dietary supplement Dexaprine Synephrine, oxilofrine, deterenol, yohimbine, caffeine, theophylline Oxilofrine content found: 1-5 mg Ultra-high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-QTOF-MS) Netherlands [50 ] 27 18 Demelverine, hordenine, N, N-dimethyl-phenethylamine, synephrine, N-methyl-β -phenethylamine, methylsynephrine Unlisted DMAA was identified in three products with concentrations ranging from 18 to 120.9 mg/daily dose, while unlisted DMBA was found in one product with a concentration of 108 mg/daily dose LC-QTOF-MS USA [51 ] 30 11 4-Androstenedione 4-Androstenedione was found in a range of 1.04 ng/g-2.52 ng/g UPLC-MS/MS Iran [53 ] 108 53 1,3-Dimethylamylamine, sibutramine, methylphenidate, synephrine DMAA was present in 20% of the dietary supplements. Out of the 108 samples, almost 50% were positive for sibutramine and 10% for methylphenidate DART-MS/MS Brazil, USA [54 ] 11 3 Sibutramine Concentrations of sibutramine ranged from 3.5 mg/g to 4.08 mg/g Electrochemiluminescence (ECL) China [55 ] 16 13 Benfluorex, fluoxetine, pseudoephedrine, tiratricol Pseudoephedrine 2.6-55.56 mg LC-UV Italy [57 ] 120 29 Sibutramine, fluoxertine Sibutramine 0.26-113.22 mg per capsule UHLPC-LTQ-Orbitrap MS China [58 ] 17 8 1,3-Dimethylamylamine (1,3-DMAA), 1,4-dimethylamylamine (1,4-DMAA), 1,3-dimethylbutylamine (1,3-DMBA), higenamine, deterenol, phenpromethamine, oxilofrine, octodrine, beta-methylphenylethylamine Concentration range for detected stimulants were 2.7-17 mg of deterenol, 1.3-20 mg of phenpromethamine, 5.7-92 mg of beta-methylphenylethylamine, 18-73 mg of octodrine, 48 mg of higenamine, 18-55 mg of oxilofrine, 17 mg of 1,3-dimethylamylamine, 1.8 mg to 6.6 of 1,3-dimethylbutylamine, and 5.3 mg of 1,4-dimethylamylamine UHPLC quadrupole-Orbitrap MS Netherlands [59 ] 32 16 Phenethylamine, synephrine, oxilofrine, hordenine, beta-methylphenethylamine, N-methyltyramine, octopamine, deterenol High concentrations of phenethylamine were found in two products (29.9 and 26.8%, respectively). Synephrine was detected in 15 products with various contents ranging from 0.5 to 5.7%. The concentration of oxilofrine in these products ranged from 0.2 to 11.6%; deterenol with a content of 4.1%. The potential intake of the compound was estimated to be 28.7 mg NMR USA [60 ] 40 32 Тestosterone propionate, testosterone phenylpropionate, testosterone isocaproate, testosterone decanoate, testosterone cypionate, testosterone undecanoate, stanozolol, drostanolone propionate, trenbolone acetate, oxymetholone, methandrostenolone Eight of the 40 samples analyzed lacked all or some of the components listed on the label NMR Brazil [61 ] 160 89 Sibutramine, fluoxetine, phenolphthalein, orlistat Sibutramine was detected in 26% of the capsules, with sibutramine concentration ranging from 0.1 to 22 mg per dosage unit (capsule). The dosages found in this study varied from 0.05 to 56 mg per capsule, with phenolphthalein 0.8 mg-29 mg per capsule fluoxetine NMR France [62 ] 48 3 Nandrolone, testosterone, dehydroepiandrosterone (DHEA), 5α -androstan-3,17-dione, 19-norandrostendione, progesterone Positive tests included substances at values ranging from 0.022 to 0.398 mg/kg Two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC–TOF-MS) Czech Republic [63 ] 20 5 Phenethylamine, N, N-diethyl phenethylamine, N-ethyl-α -ethyl-phenethylamine N-Ethyl-α -ethyl-phenethylamine was found in a range of 6.48-23.4 mg per capsule LC-MS-MS USA [64 ] 9 6 Ephedrine Ephedrine range: 1.08-3.54 mg per capsule HPLC USA [65 ] 7 7 1,3-Dimethylamylamine DMAA range from 1.1 mg/g to 32 mg/g was found UPLC-MS/MS USA [66 ] 2 2 Sibutramine, phenolphthalein 24.71 mg sibutramine and 48.20 mg phenolphthalein were found HPLC Romania [67 ] 10 3 Sibutramine, fluoxetine All three adulterate supplements were manufactured in China and labeled as food supplements containing only plants—“100% natural products” Fourier-transform infrared spectroscopy (FTIR) Romania [68 ] 20 3 Ephedrine, caffeine Ephedrine range: 31–90 mg/dose HLPC Romania [69 ] 26 18 Sildenafil, tadalafil, vardenafil 69% of the analyzed products that are found on the Romanian market turned out to be adulterated LC-MS Romania [70 ] 80 76 Diphenoxylate, tramadol, codeine, sertraline, fluoxetine Diphenoxylate and tramadol are found at concentrations of 1.4–4 mg/capsule and 67–150 mg/capsule, respectively GC-MS Iran [72 ] 138 74 Fluoxetine In comparison to supplements produced and purchased in South Africa (5194 ng/g), supplements imported and purchased in South Africa showed a greater amount of fluoxetine contamination (20052 ng/g) LC-MS South Africa [73 ] 24 16 13 anabolic steroids Amount of found substances per capsule: GC-MS UK [74 ] 198 5 Testosterone, stanozolol, 5α -hydroxylaxogenin According to the detected concentration and daily serving size, it was found that 0.34 μ g of stanozolol would be consumed per day. LC-MS/MS Korea [75 ] 36 8 Ephedrine, pseudoephedrine Ephedrine at a concentration ranging from 370 ng/g to 1000 ng/g (in one case, ephedrine was not declared in the label) pseudoephedrine in 540 ng/g LC–HRMS Italy [76 ] 52 26 Sibutramine Half of the supplements included sibutramine in levels as high as 35 mg per capsule HPLC-UV Switzerland [77 ] 124 6 Diuretics Nearly 5% of the samples were found to be contaminated with diuretics at values ranging from 0.051 to 162 mg/g UHPLC-Q-Orbitrap Republic of Korea [78 ] 3 3 Sibutramine A new method was developed for the identification and quantification of the sibutramine by HPTLC HPLC Turkey [79 ] 18 8 4-Androstene-3β ,17β -diol, 5α -androstane-3β ,17β -diol Concentration that was around or above 0.01 mg per capsule or tablet was found LC-MS/MS Netherlands [80 ] 2 2 Мetandienone, Stanozolol Metandienone with a concentration of 16.8 mg/tablet and stanozolol 14.5 mg/tablet were identified. Norandrostenedione was also found in both products, along with small levels of numerous additional steroids GC-MS Germany [81 ]
