( S i l d e n a f i l a n a l o g u e ) Homosildenafil (Sildenafil analogue ) H y d r o c h l o r o t h i a z i d e Hydroxyacetild

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1 : Ann. Rept. Food Drug Res. 3 : , % 27.4% (225/822)14.8% (303/2,042) 180.1% (423/528)216.7% (88/528) 3 N-desmethylsibutramineSibutramineCaffeine SildenafilTadalafilVardenafilSibutramine ㈠ 100 2,864 ㈡ A c e t a m i n o p h e n A c e t i l a c i d ( S i l d e n a f i l a n a l o g u e ) A c e t i l d e n a f i l ( S i l d e n a f i l analogue466)acetyl vardenafil ( Va r d e n a f i l a n a l o g u e ) Aminotadalafil (Tadalafil analogue 390)BenzylpiperazineBisacodyl BumetanideCaffeineChloramphenicol ChlorpheniramineChloropretadalafil ( Ta d a l a f i l a n a l o g u e ) ClobenzorexDehydroepiandrosterone DiclofenacDimethylsildenafil (Sildenafil a n a l o g u e ) E p h e d r i n e FenofibrateFlunitrazepamFluoxetine FurosemideGemfibrozilGendenafil

2 ( S i l d e n a f i l a n a l o g u e ) Homosildenafil (Sildenafil analogue ) H y d r o c h l o r o t h i a z i d e Hydroxyacetildenafil (Sildenafil analogue ) H y d r o x y h o m o s i l d e n a f i l ( S i l d e n a f i l a n a l o g u e ) Hydroxythiohomosildenafil (Sildenafil analogue520)imidazosagatriazinone ( S i l d e n a f i l a n a l o g u e ) L o v a s t a t i n M e l a t o n i n M e t f o r m i n MethyltestosteroneMetoclopramide N-butyltadalafil (Tadalafil analogue ) N - d e s m e t h y l s i b u t r a m i n e (Sibutramine analogue265) N-did esmethylsibutramine (Sibutramine analogue251)nicotinamide Nor-acetildenafil (Sildenafil analogue 452)Nortadalafil (Tadalafil analogue 375)OrlistatPhenolphthalein PhenylephrinePiperidenafil (Vardenafil a n a l o g u e ) P i r o x i c a m PropranololRimonabantSennosides SibutramineSildenafilSynephrine Ta d a l a f i l Te s t o s t e r o n e p r o p i o n a t e TheophyllineThiamineThioaildenafil (Sildenafil analogue504)thioctic a c i d T h i o h o m o s i l d e n a f i l ( S i l d e n a f i l analogue504)thiosildenafil (Sildenafil analogue490)vardenafil a n a l o g u e ( ) Yo h i m b i n e Zolpidem4-methylethcathinone7-ketodehydroepiandrosteroneSIGMA TLC PharmaChemCacheSyn 95% ㈢ (1-3) 1. Dragendorff s Spray Reagent 2. 50%Spray Reagent Tetrazolium Blue Spray Reagent 5. p-dimethylaminobenzaldehyde Spray Reagent 6. Ninhydrin Spray Reagent 7. Anisaldehyde-Sulfuric Acid Spray Reagent 8. 2,4-Dinitrophenylhydrazine Spray Reagent 9. p-dimethylaminocinnamaldehyde Spray Reagent 10. 5% Ferric Chloride Spray Reagent 11. Iodoplatinate Spray Reagent 12. Iodoplatinate Spray Reagent, acidified 13. 1% Mercurous Nitrate Spray Reagent 14. Potassium Permanganate Spray Reagent 15. Potassium Permanganate Spray Reagent, acidified 16. 1% Vanillin-Sulfuric Acid Spray Reagent ㈣ 1. Merck TLC plates, silica gel 60 F cm 2. Varian CARY 300 Bio spectrophotometer 3. (GC/MS)HP 6890 GC system with HP5973 mass selective detector Thermo DSQ with Thermo TRACE GC ULTRA 4. (HPLC)Agilent 1100 series with photodiode array detector Hitachi L-2000 series with photodiode array detector 5. (LC/MS/MS) Waters 2695 Alliance LC & 2998 photodiode array detector with Quattro Premier XE 95% 5 ml 5 (721 v/v)(811v/v)

3 350 (91v/v)(11v/ v)(41v/v) nm95% R f keto-dehydroepiandrosteroneCaffeine DehydroepiandrosteroneSynephrine ( 100 )() ,042 2, (%) 件數 ( 年度服務案件抽查案件合計檢出率 (%) 年度服務案件抽查案件合計 ,441 2, (%)

4 )4 () 15.9% ( %) 17.1%( 46.2%)(26.7%)(21.8%) 1, % 20.2% (4-9) 100 種類數各年度檢出西藥種類數年度平均個數 N-desmethylsibutramine 2 62 Sibutramine 3 50 Caffeine 4 49 Aminotadalafil 4 49 Tadalafil 5 41 Phenolphthalein 5 41 Sildenafil 6 39 Thioaildenafil 7 38 Sennosides 8 26 Nortadalafil 9 14 Acetil acid 9 14 Dimethylsildenafil N-didesmethylsibutramine Nor-acetildenafil Acetildenafil Melatonin 13 9 Hydroxyhomosildenafil 13 9 Hydroxythiohomosildenafil 13 9 Yohimbine 14 7 Bisacodyl 14 7 Fluoxetine 15 6 Piperidenafil 16 5 Gendenafil 16 5 Synephrine 17 4 Gemfibrozil 17 4 Thiosildenafil 18 3 Furosemide 18 3 Imidazosagatriazinone 每件檢出檢體平均含西藥成分個數年度

5 () 18 3 Lovastatin ketodehydroepiandrosterone 19 2 Acetyl vardenafil 19 2 Chlorpheniramine 19 2 Clobenzorex 19 2 Fenofibrate 19 2 Hydrochlorothiazide 19 2 Hydroxyacetildenafil 19 2 Metformin 19 2 Methyltestosterone 19 2 Metoclopramide 19 2 Propranolol 19 2 Vardenafil analogue ( 312) methylethcathinone 20 1 Acetaminophen 20 1 Benzylpiperazine 20 1 Bumetanide 20 1 Chloramphenicol 20 1 Chloropretadalafil 20 1 Dehydroepiandrosterone 20 1 Diclofenac 20 1 Ephedrine 20 1 Flunitrazepam 20 1 Homosildenafil 20 1 N-butyltadalafil 20 1 Nicotinamide 20 1 Orlistat 20 1 Phenylephrine 20 1 Piroxicam 20 1 Rimonabant 20 1 Testosterone propionate 20 1 Theophylline 20 1 Thiamine 20 1 Thioctic acid 20 1 Thiohomosildenafil 20 1 Zolpidem (10,11) N-desmethylsibutramineSibutramineCaffeine AminotadalafilTadalafil 64 23Aminotadalafil Tadalafil49Sildenafil 41Thioaildenafil ( )10 N-desmethylsibutramine63Sibutramine 62Phenolphthalein Sennosides(Sennoside AB )12 mg (1-3) (528) 49.1% (259/528)46.4% (245/528) 100.0% (1/1)30.2% (245/812)19.5% (259/1,328) 2, % (1,328/2,864)28.4% (812/2,864)11.6% (332/2,864) 74.7% (2,140/2,864)

6 Acetil acid Acetildenafil Acetyl vardenafil 2 Aminotadalafil Carbodenafil 1 Chloropretadalafil 1 Dimethylsildenafil Gendenafil Homosildenafil Hydroxyacetildenafil Hydroxyhomosildenafil Hydroxythiohomosildenafil Imidazosagatriazinone 3 N-butyltadalafil 1 Nor-acetildenafil 6 11 Nortadalafil 26 Piperidenafil Sildenafil Tadalafil Thioaildenafil Thiohomosildenafil Thiosildenafil Vardenafil Vardenafil analogue (312) Vardenafil analogue (437) 2 Yohimbine Clobenzorex N-Desmethylsibutramine N-Didesmethylsibutramine Orlistat 1 Phenolphthalein Rimonabant Sennosides Sibutramine

7 / (%) / (%) / (%) 1 259/ 528 (49.1) 259/ 1,328 (19.5) 1,328/ 2,864 (46.4) 2 245/ 528 (46.4) 245/ 812 (30.2) 812/ 2,864 (28.4) 3 12/ 528 (2.3) 12/ 64 (18.8) 64/ 2,864 (2.2) 4 4/ 528 (0.8) 4/ 332(1.2) 332/ 2,864 (11.6) 5 2/ 528 (0.4) 2/ 32 (6.3) 32/ 2,864 (1.1) 5 2/ 528 (0.4) 2/ 26 (7.7) 26/ 2,864 (0.9) 7 1/ 528 (0.2) 1/ 56 (1.8) 56/ 2,864 (2.0) 7 1/ 528 (0.2) 1/ 1 (100.0) 1/ 2,864 (0.0) 7 1/ 528 (0.2) 1/ 10 (10.0) 10/ 2,864 (0.3) 7 1/ 528 (0.2) 1/ 32 (3.1) 32/ 2,864 (1.1) /(%) %2 16.7% 4 1 SildenafilHydroxyacetildenafilHydroxyhomosildenfilHydroxythiohomosildenfil ( ) 21.1% (367/1,743)15.6% (82/524)9.8% (36/368) 40.0% (4/10) 28.9% (35/121)

8 , (%) , , %14.8%2, % 30% 88 SildenafilTadalafilVardenafil Sildenafil14 (12,13,18) Acetil acid (356) Acetildenafil (466)Carbodenafil ( 452)Dimethylsildenafil (488) Gendenafil (354)Homosildenafil (488)Hydroxyacetildenafil ( 482)Hydroxyhomosildenafil (504) Hydroxythiohomosildenafil (520) Imidazosagatriazinone (312)Noracetildenafil (452)Thioaildenafil (504)Thiohomosildenafil ( 504)Thiosildenafil (490) Tadalafil4 (17) Aminotadalafil (390)Chloropretadalafil ( 426)N-butyltadalaf il (431) Nortadalaf il (375)Vardenafil 4 (14,15) Acetyl vardenafil ( 466)Piperidenafil (459)Vardenafil analogue (312)Vardenafil analogue (437) 2291 Homosildenafil93Acetildenafil Hydroxyhomosildenafil 294 GendenafilAminotadalafil Piperidenafil395 Vardenafil(312)96 Hydroxyacetildenafil97 Vardenafil(437) 98Acetil acidcarbodenafil HydroxythiohomosildenafilThioaildenafil ThiohomosildenafilThiosildenafil6 99DimethylsildenafilNoracetildenafil 2Acetyl vardenafil ChloropretadalafilImidazosagatriazinone N-butyltadalafilNortadalafil100 S i l d e n a f i l Ta d a l a f i l VardenafilSildenafil TadalafilVardenafil SAR

9 Sibutramine62 SibutramineN-Desmethylsibutramine (265) (16) N-Didesmethylsibutramine (251) Sibutramine Clobenzorex OrlistatRimonabantSennosides Rimonabant Clobenzorex Clobenzorex Clobenzorex Phenolphthalein () () () ()() : : : : : : Lai, K. C., Liu, Y. C., Tseng, M. C. and Lin, J. H.

10 Isolation and identification of a sildenafil analogue illegally added in dietary supplements. J. Food Drug Anal. 14: Lin, M. C., Liu, Y. C. and Lin, J. H Identification of a sildenafil analogue adulterated in two herbal food supplements. J. Food Drug Anal. 14: Lai, K. C., Liu, Y. C., Tseng, M. C., Lin, Y. L. and Lin, J. H Isolation and identification of a vardenafil analogue in a functional food marketed for penile erectile dysfunction. J. Food Drug Anal. 15: Lai, K. C., Liu, Y. C., Tseng, M. C., Lin, Y. L. and Lin, J. H Isolation and identification of a vardenafil analogue in a dietary supplement. J. Food Drug Anal. 15: Lai, K. C., Liu, Y. C., Tseng, M. C., Lin, Y. L. and Lin, J. H Isolation and identification of a sibutramine analogue in a healthy food for weight loss. J. Food Drug Anal. 15: Lin, M. C., Liu, Y. C., Lin, Y. N. and Lin, J. H Identification of a tadalafil analogue adulterated in a dietary supplement. J. Food Drug Anal. 17: Lai, K. C., Liu, Y. C., Liao, Y. C., Lin, Y. L., Tsai, L. Y., Lin, J. H. and Lo, C. F Isolation and identification of three thio-sildenafil analogues in dietary supplements. J. Food Drug Anal. 18: Survey on Pharmaceutical Adulterants in Dietary Supplements in the Fiscal Year 2011 YOE-RAY KU, LI-YAO TSAI, MEI-CHIH LIN, YA-HUI HSU, KUO-CHIN LAI, KANG-TSU LU, HUI-CHUN LEE, YI-CHU LIU, DANIEL YANG-CHIH SHIH AND CHI-FANG LO Division of Research and Analysis, FDA ABSTRACT In this report, the survey results were presented for the pharmaceutical adulterants in 2,864 samples of marketed dietary supplements, which were collected and analyzed during the year The results indicated that 27.4% (225/822) of the samples from the consumer service centers of the local health bureaus and other government institutions were adulterated with pharmaceutical compounds. Other samples, which were randomly collected from markets by the local health officers, had an adulteration rate of 14.8% (303/2,042). Among the 528 samples containing adulterants, 80.1% contained 1 adulterant and 16.7% 2 adulterants. In terms of usage, most of adulterants were used for anorexic or male erectile dysfunction. As the frequency of occurance was concerned, N-desmethylsibutramine, sibutramine and caffeine ranked the top. In addition to commercial sildenafil, tadalafil, vardenafil and sibutramine, 22 analogues of these drugs were found. Key words: adulterants in dietary supplements, erectile dysfunction, anorexic

M e t h y l e p h e d r i n e M e t o c l o p r a m i d e N-desmethylsibutramine (Sibutramine a n a l o g u e ) N-didesmethylsibutramine

M e t h y l e p h e d r i n e M e t o c l o p r a m i d e N-desmethylsibutramine (Sibutramine a n a l o g u e ) N-didesmethylsibutramine 196. 4 : 196-205 2013 Ann. Rept. Food Drug Res. 4 : 196-205 2013 101 101TFDA 1,872270 14.4% 409125 (30.6%) 1,463145 (9.9%) 72685 (11.7%)542168 (31.0%) 3Sildenafil Sibutramine Tadalafil Sildenafil Tadalafil