213 C h l o r d i a z e p o x i d e, C h l o r p h e n i r a m i n e, Chlorzoxazone, Cimetidine, Clobenzorex, Dexamethasone, Dextromethorphan, Diazepa

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1 : Ann. Rept. Food Drug Res. 1 : % 34465(18.9%)16957(33.7%) 25635(13.7%) 25787(33.9%) (46.7%)3514(11.5%) 3Caffeine AcetaminophenHydrochlorothiazide (1-3) (4-23) (24-28) (29-42) 6.0~26.4%98 ㈠㈡ Acetaminophen, Bromhexine, Bromisovalum, Caffeine, Carbinoxamine,

7%) 25635(13.7%) 25787(33.9%)122157 (46.7%)3514(11.

2 213 C h l o r d i a z e p o x i d e, C h l o r p h e n i r a m i n e, Chlorzoxazone, Cimetidine, Clobenzorex, Dexamethasone, Dextromethorphan, Diazepam, Diclofenac, Dicyclomine, Diphenhydramine, Diprophylline, Guaiacol glyceryl ether, Hydrochlorothiazide, Ibuprofen, Indomethacin, Mefenamic acid, Methylparaben, Nitrazepam, Papaverine, Phenylpropanolamine, Piroxicam, Prednisolone, Propyphenazone, Sibutramine, Sildenafil, Sulfathiazole, Sulindac, Thiamine HCl, Thiamine disulfide, Triprolidine SIGMA Ethoxybenzamide NACALAI TESQUEAcetildenafil, Desmethylsibutramine, Piperidenafil, Sildenafil, Ta d a l a f i l Va r d e n a f i l T L C PHARMA CHEMVardenafil analogue (312) (NMR) (MS) Lab-scan()R.D.H. ()Merck() 95% ㈢ Dragendorff s spray reagent, 50% Sulfuric Acid- Ethanol spray reagent, Iodine vapor, Tetrazolium blue spray reagent, p-dimethylaminobenzald ehyde spray reagent, Ninhydrin spray reagent, Anisaldehyde-Sulfuric Acid spray reagent, 2,4- Dinitrophenylhydrazine spray reagent, p-dim ethylaminocinnamaldehyde spray reagent, 5% Ferric Chloride spray reagent, Iodoplatinate spray reagent, Iodoplatinate (acidified) spray reagent, 1% Mercurous Nitrate spray reagent, Potassium Permanganate spray reagent, Potassium Permanganate (acidified) spray reagent, 1% Vanillin-Sulfuric Acid spray reagent. ㈣: 1. : MerckTLC plates silica gel 60 F x 20 cm 2. : Varian CARY 300 Bio 3. (GC/MS): (1) HP 6890 GC system with HP 5973 mass selective detector (2) T h e r m o T R A C E G C U l t r a w i t h autosampler AS 3000 and mass DSQ 4. (HPLC): Hitachi L-2000 series with photodiode array detector 5. (LC/MS/MS): Waters 2690 Alliance LC & 991 photodiode array detector with Micromass Quattro Ultima 95% 30 (7 : 2 : 1v/v) (8 : 1 : 1v/v) (9 : 1v/v)(1 : 1v/v) (4 : 1v/v) 254 nm 366 nm 95% R f

Propyphenazone, Sibutramine, Sildenafil, Sulfathiazole, Sulindac, Thiamine HCl, Thiamine disulfide, Triprolidine SIGMA Ethoxybenzamide NACALAI TESQUEAcetildenafil, Desmethylsibutramine,

3 (29-42) (18.9%) 16957(33.7%) % %23.8% (34-42) 89 (34) (%) ( ) 13.7% % % (%)

6%16825 14.9% (%) 40 35 33.7 30 28.6 25 24.3 22.3 23.8 20 15 18.1 15.1 17.0 15.3 20.3 13.4 16.

4 () () (%) (%) 年度 ( ) (%) 國術館青草店非專業人員其它年度 ( )

8 80 (%) 70 60 50 40 30 20 10 0 89 90 91 92 93 94 95 96 97 98 年度 89 98 ( )

5 % (48.6%) % 年度年度 89 98

90 91 92 93 94 95 96 97 98 年度 89 98 10.00 4.40 3.54 3.73 3.

6 CaffeineAcetaminophen Hydrochloro-thiazideIndomethacinSildenafil Chlorphe-niramineEthoxybenzamidePiroxicam () (1) (122) 28.7% (35/122)15.6% (19/122)13.9% (17/122) 13.1% (16/122)8.2% (10/122) 6.6% (8/122)4.1% (5/122) 2.5% (3/122)2.5% (3/122) 1.6% (2/122)1.6% (2/122) 0.8% (1/122) % % Caffeine 19 3 Mefenamic acid 2 39 Acetaminophen 19 3 Carbinoxamine 3 32 Hydrochlorothiazide 19 3 Prednisolone 4 24 Indomethacin 19 3 Bromhexine 5 21 Sildenafil 19 3 * Piperidenafil 6 16 Chlorpheniramine 20 3 * Desmethylsibutramine 7 13 Ethoxybenzamide 30 2 Papaverine 8 11 Piroxicam 30 2 Cimetidine 9 8 Chlorzoxazone 32 1 Diclofenac 10 7 Dicyclomine 32 1 Triprolidine 10 7 Vardenafil 32 1 Sulindac 12 6 Tadalafil 32 1 Propyphenazone 12 6 Guaiacol glyceryl ether 32 1 Sulfathiazole 12 6 Chlordiazepoxide 32 1 * Acetildenafil 12 6 Dextromethorphan 32 1 Phenylpropanolamine 15 5 Ibuprofen 32 1 Nitrazepam 15 5 Diazepam 32 1 Diphenhydramine 15 5 Sibutramine 32 1 Dexamethasone 19 3 * Vardenafil analogue (M.W.312) 32 1 Diprophylline 19 3 Thiamine Disulfide 32 1 Clobenzorex 19 3 Thiamine HCl 32 1 Bromisovalum 19 3 Methylparaben *98

5%2 98 1 53 Caffeine 19 3 Mefenamic acid 2 39 Acetaminophen 19 3 Carbinoxamine 3 32 Hydrochlorothiazide 19 3 Prednisolone 4 24 Indomethacin 19 3 Bromhexine 5 21 Sildenafil 19 3 * Piperidenafil 6 16

7 /(%) 1 35/122 (28.7) 2 19/122 (15.6) 3 17/122 (13.9) 4 16/122 (13.1) 5 10/122 (8.2) 6 8/122 (6.6) 7 5/122 (4.1) 8 3/122 (2.5) 8 3/122 (2.5) 10 2/122 (1.6) 10 2/122 (1.6) 12 1/122 (0.8) 12 1/122 (0.8) / (%) %49.8%6 75.7%4.1% Acetaminophen, Bromhexine, Caffeine, Chlorpheniramine, Dextromethorphan, EthoxybenzamideGuaiacol glyceryl ether % (54/251)27.2% (40/147) 36.1% (22/61) % % (%)

.8%6 75.7%4.1% Acetaminophen, Bromhexine, Caffeine, Chlorpheniramine, Dextromethorphan, EthoxybenzamideGuaiacol glyceryl ether 7 1 98 21.5% (54/251)27.2% (40/147) 36.

8 % 985 SildenafilTadalafilVardenafil % 33.9% 98 SildenafilVardenafilTadalafil Acetildenafil (466) Vardenafil analogue (312)Piperidenafil( ) 9 8 SibutramineDesmethylsibutramine (265) Sildenafil TadalafilVardenafilSibutramine (72~98) 1991 () 1995

analogue (312)Piperidenafil( 4 5 9 ) 9 8

9 220 () () ()() 4. Ku, Y. R., Tsai, M. J. and Wen, K. C Screening chemical drugs used to adulterate in rheumatic and analgesic traditional Chinese medicine by HPLC-DAD. J. Food Drug Anal. 3: Ku, Y. R., Tsai, M. J. and Wen, K. C Determination of sulfamethoxazole adulterated in traditional Chinese medicine. J. Food Drug Anal. 3: Ku, Y. R., Tsai, M. J. and Wen, K. C Study on the adulterated chemical drugs in rheumatic and analgesic traditional Chinese medicine by MEKC. J. Food Drug Anal. 3: Lai, S. J., Binder, S. R., Essien, H. and Wen, K. C Identification of western medicines as adulterated in Chinese herbal medicines using a broad-spectrum drug screening HPLC system. J. Lig. Chromatogr. 18: T s e n g, M. C., T s a i, M. J. a n d We n, K. C Q u a n t i t a t i v e a n a l y s i s o f acetaminophen, ethoxybenzamide, piroxicam, hydrochlorothiazide, caffeine, chlorzoxazone and nicotinamide illegally adulterated in Chinese medicinal pills. J. Food Drug Anal. 4: Ku, Y. R., Tsai, M. J. and Wen, K. C Determination of aminitrozole, metronidazole, ornidazole and tinidazol adulterated in traditional Chinese medicine by high performance liquid chromatography. J. Food Drug Anal. 4: Song, Y., Her, G. R. and Wen, K. C Analysis of synthetic drugs in adulterated Chinese medicine by high performance liquid chromatography/electrospray mass spectrometry. J. Food Drug Anal. 5: Ku, Y. R., Tsai, M. J., Lin, J. H. and Wen, K. C Micellar electrokinetic capillary chromatography of clobenzorex HCl and diazepam adulterated in anorexiant traditional Chinese medicine. Chin. Pharm. J. 48: Ku, Y. R., Tsai, M. J. and Wen, K. C Quantitative analysis of nifedipine adulterated in traditional Chinese medicine by HPLC. Formosa J. Clin. Pharm. 5: Ku, Y. R., Tsai, M. J. and Wen, K. C Determination by high performance liquid c h r o m a t o g r a p h y o f f l u o x y m e s t e r o n e, methyltestosterone and testosterone adulterated in Chinese herbal preparations. J. Food Drug Anal. 5: Huang, W. F., Wen, K. C. and Hsiao, M. L Adulteration by synthetic therapeutic substances of traditional Chinese medicines in Taiwan. J. Clin. Pharmacol. 37: Ku, Y. R., Wen, K. C., Ho, L. K. and Chang, Y. S Determination of xanthine bronchodilators in adulterated Chinese herbal preparations by high performance liquid chromatography. Chin. Pharm. J. 50: Ku, Y. R., Wen, K. C., Ho, L. K. and Chang, Y. S Solid-phase extraction and high performance liquid chromatographic determination of steroids adulterated in traditional Chinese medicine. J. Food Drug Anal. 7: Ku, Y. R., Wen, K. C., Ho, L. K. and Chang, Y. S Solid-phase extraction for the determination of caffeine in traditional Chinese medicinal prescriptions containing Theae Folium by high performance liquid chromatography. J. Pharm. Biomed. Anal. 20: Ku, Y. R., Wen, K. C., Ho, L. K. and Chang, Y. S Analysis and confirmation of synthetic anorexics in adulterated by high performance capillary electrophoresis. J. Chromatogr. A. 848:

J. Food Drug Anal. 3: 185-192. 7. Lai, S. J., Binder, S. R., Essien, H. and Wen, K. C. 1995.

10 Tseng, M. C., Tsai, M. J., Lin, J. H. and Wen, K. C GC/MS analysis on anorectics adulterated in traditional Chinese medicines. J. Food Drug Anal. 8: Lin, M. C., Lin, J. H. and Wen, K. C Detection and determination of phenformin in Chinese medicinal capsules by GC-MS and HPLC. J. Food Drug Anal. 9: Ku, Y. R., Liu, Y. C. and Lin, J. H Solid-phase extraction and high performance liquid chromatographic analysis of prednisone adulterated in a foreign herbal medicine. J. Food Drug Anal. 9: Ku, Y. R., Liu, Y. C. and Lin, J. H Highperformance liquid chromatographic analysis of sildenafil citrate and methyltestosterone adulterated in a herbal medicine, The Chinese Pharmaceutical Journal, 54: Ku, Y. R., Chang, L. Y., Ho, L. K. and Lin, J. H Analysis of synthetic antidiabetic drugs in adulterated traditional Chinese medicines by high-performance capillary electrophoresis, J. of Pharm. and Biomed. Analy. 33: 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. 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 sibutramine analogue in a healthy food for weight loss 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 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: : : : : : : : : : : :

Solid-phase extraction and high performance liquid chromatographic analysis of prednisone adulterated in a foreign herbal medicine. J. Food Drug Anal. 9: 150-152. 22. Ku, Y. R., Liu, Y. C. and Lin, J.

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12 223 Survey on Adulterants in Chinese Medicinal Preparations during the Fiscal Year 2009 KUO-CHIH LAI 1, YUNG-CHIH LIAO 1, MEI-CHIH LIN 1, YOE-RAY KU 1, LI-YAO TSAI 1, HUI-CHUN LEE 1, ZENG-YI FAN 2, YI-TING WANG 3, YI-CHU LIU 1, JER-HUEI LIN 1 AND CHI-FANG LO 1 1 Division of Research and Analysis, 2 Division of Planning and Research Development, 3 Central Center for Regional Administration ABSTRACT In order to investigate the chemical compound adulteration in Chinese medicinal preparations (CMP), 513 samples were collected and analyzed during the fiscal year of The result showed that 18.9% (65/344) of the samples acquired from the consumer service centers of the local health bureaus and judicial organizations were adulterated. However, if the samples that collected by local health bureau from local markets were included, the adulteration rate increased to 23.8% (122/513). The sources of samples were classified into two categories. The first one were collected from legal institutions, including manufacturers of CMP and medical units such as hospitals, clinics and dealers of traditional Chinese medicine, in which the average adulterated rate was 13.7%. The second one were from illegal suppliers, such as Chinese kung-fu stores, folk medicine stores, unlicensed practitioners and others, where the average adulterated rate was 33.9%. One hundred and twenty two samples contained adulterants, among them, 46.7% with 1 adulterant, 11.5% with 3 or 5 adulterants. In terms of therapeutic activity, most adulterants found in the CMP were for treatment of erectile dysfunction. The therapeutic activity of most adulterants was irrelevant to the claimed use of CMP. The result also showed that caffeine was the mostly found constituents in adulterants, the other were acetaminophen and hydrochlorothiazide. Key words: adulterants, Chinese medicinal preparations

ABSTRACT In order to investigate the chemical compound adulteration in Chinese medicinal preparations (CMP), 513 samples were collected and analyzed during the fiscal year of 2009.

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