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

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1 : Ann. Rept. Food Drug Res. 4 : TFDA 1, % (30.6%) 1, (9.9%) (11.7%) (31.0%) 3Sildenafil Sibutramine Tadalafil Sildenafil Tadalafil Vardenafil Sibutramine 16 TFDA TFDA101 ㈠ 101TFDA 1,872 ㈡ A c e t a m i n o p h e n Aminophylline Aminotadalafil (Tadalafil analogue390) Amphetamine Aspirin Benzbromarone Caffeine Chloropretadalafil (Tadalafil analogue 426) Chlorpheniramine Cetilistat Clobenzorex Dehydroepiandrosterone Dexamethasone Dextromethorphan Diazepam Dithiodesmethylcarbodenafil ( S i l d e n a f i l a n a l o g u e ) E p h e d r i n e H y d r o c h l o r o t h i a z i d e Hydroxyhomosildenafil (Sildenafil analogue ) I n d o m e t h a c i n M D M A ( 3, 4 - M e t h y l e n e d i o x y m e t h a m p h e t a m i n e ) M e f e n a m i c a c i d M e l a t o n i n

2 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 (Sibutramine analogue251) N-ethyltadalafil (Tadalafil analogue403) Noracetildenafil (Sildenafil analogue 452) Nortadalafil (Tadalafil analogue 375) Orlistat Phenolphthalein Phenylpropanolamine Piperidenafil (Vardenafil a n a l o g u e ) P i r o x i c a m Prednisolone Propoxyphenylaildenafil ( 502) Pseudoephedrine Sennoside A B Sibutramine Sildenafil Sildenafil analogue ( 484) Sildenafil analogue ( 518) Sildenafil analogue ( 534) Synephrine Tadalafil Thioaildenafil ( S i l d e n a f i l a n a l o g u e ) 1,4-DibenzylpiperazineSIGMA TLC PharmaChem CacheSyn 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. (Silica Gel 60 F 254, Merck, Germany) 2. (CARY 300 Bio, Varian, USA) 3. (7693 Autosampler, 7890A GC system, 5975C inert XL MSD with Triple Axis Detector, Agilent, USA) 4. (AS 3000 Autosampler, Trace GC Ultra with DSQ, Thermo, USA) 5. (AS 3000 Autosampler, Trace GC Ultra with POLARIS Q, Thermo, USA) 6. (1100 series, Agilent, USA) 7. (L-2000 series, Hitachi, Japan) 8. (2695 Alliance LC, 2998 Photodiode Array Detector with Quattro Premier XE, Waters, USA) 195% 5 (7 2 1 v/v) (8 1 1 v/v)(9 1 v/ v)(1 1 v/v) (4 1 v/v) nm 95% R f

3 198 TFDATFDA 101 Caffeine Synephrine 1,4-Dibenzylpiperazine ( ) ( ) 101 () ( ) 3 () () (11-12) ( ) Sildenafil Sibutramine Tadalafil Phenolphthalein 409 1,463 1, % Sildenafil 65 Tadalafil28 Dithiodesmethylcarbodenafil Nortadalafil ( )9 Sibutramine32Phenolphthalein27 N-desmethylsibutramine %

4 Sildenafil 2 32 Sibutramine 3 28 Tadalafil 4 27 Phenolphthalein 5 19 Dithiodesmethylcarbodenafil 5 19 Nortadalafil 6 18 Caffeine 7 16 Aminotadalafil 8 14 N-desmethylsibutramine 9 12 Hydroxythiohomosildenafil 9 12 Sennosides 10 9 N-didesmethylsibutramine 11 7 Thioaildenafil 12 6 Propoxyphenylaildenafil ( 502) 12 6 Sildenafil analogue ( 534) 13 5 N-ethyltadalafil 13 5 Sildenafil analogue ( 484) 13 5 Sildenafil analogue ( 518) 14 4 Chloropretadalafil 14 4 Cetilistat 14 4 Melatonin 15 3 Acetaminophen 15 3 Synephrine ,4-dibenzylpiperazine 16 2 Benzbromarone 16 2 Ephedrine 16 2 Hydrochlorothiazide 16 2 Hydroxyhomosildenafil 16 2 Indomethacin 16 2 Methylephedrine 16 2 Orlistat 16 2 Piperidenafil 17 1 Aminophylline 17 1 Amphetamine 17 1 Aspirin 17 1 Chlorpheniramine 17 1 Clobenzorex 17 1 Dehydroepiandrosterone

5 ( ) 17 1 Dexamethasone 17 1 Dextromethorphan 17 1 Diazepam 17 1 MDMA 17 1 Mefenamic acid 17 1 Metoclopramide 17 1 Noracetildenafil 17 1 Phenylpropanolamine 17 1 Piroxicam 17 1 Prednisolone 17 1 Pseudoephedrine Sennosides(Sennoside A B ) 12 mg 12 mg 12 mg (1-3) (270 ) ()62.2% (168/270) 31.5% (85/270) (1,872 )3 38.8% (726/1,872)29.0% (542/1,872) 12.7% (238/1,872) 67.7% (1,268/1,872) 101 / (%) ()1 74.8%2 19.6% () () () / (%) 1 168/270 (62.2) 542/1,872 (29.0) 2 85/270 (31.5) 726/1,872 (38.8) 3 4/270 (1.5) 46/1,872 (2.5) 4 3/270 (1.1) 30/1,872 (1.6) 4 3/270 (1.1) 40/1,872 (2.1) 5 2/270 (0.7) 4/1,872 (0.2) 5 2/270 (0.7) 238/1,872 (12.7) 6 1/270 (0.4) 24/1,872 (1.3) 6 1/270 (0.4) 28/1,872 (1.5) 6 1/270 (0.4) 6/1,872 (0.3)

6 / (%) 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 , % TFDA ( ) 9.9% Caffeine Dexamethasone Hydrochlorothiazide Indomethacin Metoclopramide 88 Sildenafil Tadalafil Vardenafil SAR 101 Sildenafil 19 (13-14, 19) Acetil acid ( 356)

7 Acetil acid Acetildenafil Acetyl vardenafil 2 Aminotadalafil Carbodenafil 1 Chloropretadalafil 1 4 Dimethylsildenafil Dithiodesmethylcarbodenafil * 19 Gendenafil Homosildenafil Hydroxyacetildenafil Hydroxyhomosildenafil Hydroxythiohomosildenafil Imidazosagatriazinone 3 N-butyltadalafil 1 N-ethyltadalafil * 5 Nor-acetildenafil Nortadalafil Piperidenafil Sildenafil Propoxyphenylaildenafil * 6 Sildenafil analogue ( 484) * 5 Sildenafil analogue ( 518) * 5 Sildenafil analogue ( 534) * 6 Tadalafil Thioaildenafil Thiohomosildenafil Thiosildenafil Vardenafil Vardenafil analogue ( 312) Vardenafil analogue ( 437) 2 Yohimbine Acetildenafil ( 466) Carbodenafil ( 452) Dimethylsildenafil ( 488) Dithiodesmethylcarbodenafil ( 470) Gendenafil ( 354) Homosildenafil ( 488) Hydroxyacetildenafil ( 482) Hydroxyhomosildenafil (

8 Cetilistat * 4 Clobenzorex N-Desmethylsibutramine N-Didesmethylsibutramine Orlistat 1 2 Phenolphthalein Rimonabant Sennosides Sibutramine ) Hydroxythiohomosildenafil ( 520) Imidazosagatriazinone ( 312) Nor-acetildenafil ( 452) Propoxyphenylaildenafil ( 502) Sildenafil analogue ( 484) Sildenafil analogue ( 518) Sildenafil analogue ( ) T h i o a i l d e n a f i l ( 504) Thiohomosildenafil ( 504) Thiosildenafil ( 490) Tadalafil 5 (18) Aminotadalafil ( 390) Chloropretadalafil ( 426) N-butyltadalafil ( 431) N-ethyltadalafil ( 403) Nortadalafil ( 375) Va r d e n a f i l 4 (15-16) A c e t y l vardenafil ( 466) Piperidenafil ( 459) Vardenafil analogue ( 312) Vardenafil analogue ( 437) 2891 Homosildenafil 93Acetildenafil Hydroxyhomosildenafil 94 Gendenafil Aminotadalafil Piperidenafil 9 5 Va r d e n a f i l ( 312) 96Hydroxyacetildenafil 9 7 V a r d e n a f i l ( ) 9 8 A c e t i l a c i d Carbodenafil Hydroxythiohomosildenafil Thioaildenafil Thiohomosildenafil Thiosildenafil 99Dimethylsildenafil N o r - a c e t i l d e n a f i l Acetyl vardenafil Chloropretadalafil Imidazosagatriazinone N-butyltadalafil Nortadalafil Dithiodesmethylcarbodenafil N-ethyltadalafil Propoxyphenylaildenafil ( 502) Sildenafil( 484) Sildenafil( 518) Sildenafil ( 534) Sibutramine32 SibutramineN-Desmethylsibutramine ( 265) (17) N-Didesmethylsibutramine ( ) Cetilistat Clobenzorex Orlistat Phenolphthalein Sennosides ㈠Phenolphthalein 96 Sibutramine 99

9 204 ㈡Cetilistat FDA Cetilistat ㈢Clobenzorex Clobenzorex Sildenafil Tadalafil Vardenafil Sibutramine ( ) ( ) ( ) ( )( ) : : : : : : : Lai, K. C., Liu, Y. C., Tseng, M. C. and Lin, J. H 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

10 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 2012 YOE-RAY KU, LI-YAO TSAI, MEI-CHIH LIN, YA-HUI HSU, KANG-TSU LU, HUI-CHUN LEE, KUO-CHIN LAI,YI-CHU LIU,YU-PEN CHEN, LIH-CHING CHIUEH AND DANIEL YANG-CHIH SHIH Division of Research and Analysis, FDA ABSTRACT In this report, the survey results were presented for the pharmaceutical adulterants in 1,872 samples of marketed dietary supplements, which were collected and analyzed during the year The results indicated that 30.6% (125/409) 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 the markets by the local health officers, had an adulteration rate of 9.9% (145/1,463). Among the 270 samples containing adulterants, 74.8% contained 1 adulterant and 19.6% contained 2 adulterants. In terms of usage, most of the adulterants were used for weight loss or erectile dysfunction. As far as the frequency of occurrence was concerned, sildenafil, sibutramine and tadalafil ranked the top. In addition to commercial sildenafil, tadalafil, vardenafil and sibutramine, 16 analogues of these drugs were found. Key words: adulterants in dietary supplements, erectile dysfunction, weight loss

( 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

( 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 348. 3 : 348-357 2012 Ann. Rept. Food Drug Res. 3 : 348-357 2012 100 1002,864 52818.4% 27.4% (225/822)14.8% (303/2,042) 180.1% (423/528)216.7% (88/528) 3 N-desmethylsibutramineSibutramineCaffeine SildenafilTadalafilVardenafilSibutramine22