212. 1 : 212-223 2010 Ann. Rept. Food Drug Res. 1 : 212-223 2010 1 1 1 1 1 1 2 3 1 1 1 1 2 3 98 51312223.8% 34465(18.9%)16957(33.7%) 25635(13.7%) 25787(33.9%)122157 (46.7%)3514(11.5%) 3Caffeine AcetaminophenHydrochlorothiazide (1-3) (4-23) (24-28) 7297 1427 (29-42) 6.0~26.4%98 ㈠ 98 513 ㈡ Acetaminophen, Bromhexine, Bromisovalum, Caffeine, Carbinoxamine,
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 254 20 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
214 98 (29-42) 344 65(18.9%) 16957(33.7%) 34465 18.9%16957 33.7%23.8%98 8997 (34-42) 89 (34) 8878912 98 344 169 513 65 57 122 (%) 18.9 33.7 23.8 ( ) 13.7%86 10 11.6%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 16.0 13.6 15.7 20.4 19.7 18.6 13.7 18.9 10 5 6.7 11.2 10.3 7.9 8.8 11.2 9.9 12.6 9.1 7.5 8.8 0 89 90 91 92 93 94 95 96 97 98 89 98
215 98 () () 0 168 86 2 256 35 10 0 212 257 513 0 25 10 0 35 17 2 0 68 87 122 (%) 0.0 14.9 11.6 0 13.7 48.6 20.0 0 32.1 33.9 23.8 80 (%) 70 60 50 40 30 20 10 0 89 90 91 92 93 94 95 96 97 98 年 度 89 98 ( ) (%) 100 90 國 術 館 青 草 店 80 70 非 專 業 人 員 其 它 60 50 40 30 20 10 0 89 90 91 92 93 94 95 96 97 98 年 度 89 98 ( )
216 33.9% (48.6%) 212 6832.1% 98 98 43 317 122 2.6 80 70 60 50 40 51 49 52 52 32 46 43 56 39 43 30 20 10 0 89 90 91 92 93 94 95 96 97 98 年 度 89 98 10.00 4.40 3.54 3.73 3.39 2.21 3.47 3.40 3.10 2.88 2.60 1.00 89 90 91 92 93 94 95 96 97 98 年 度 89 98
217 43 317122 2.6 108 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) 1 46.7%3 511.5%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 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
218 98 /(%) 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) 98 57 13 14 12 14 7 5 / (%) 46.7 10.7 11.5 9.8 11.5 5.7 4.1 10.7%49.8%6 75.7%4.1% Acetaminophen, Bromhexine, Caffeine, Chlorpheniramine, Dextromethorphan, EthoxybenzamideGuaiacol glyceryl ether 7 1 98 21.5% (54/251)27.2% (40/147) 36.1% (22/61) 28 5 1 1 5 1 8 3 2 4 2 1 2 3 2 3 1 1 2 2 5 3 2 5 1 2 1 1 6 2 2 3 3 3 1 1 2 1 1 98 513122 23.8%34465 18.9%169 98 251 147 12 61 3 12 4 16 2 5 54 40 1 22 0 0 0 2 2 1 (%) 21.5 27.2 8.3 36.1 0.0 0.0 0.0 12.5 100 20.0
219 5733.7% 985 SildenafilTadalafilVardenafil 12 98 13.7% 33.9% 98 SildenafilVardenafilTadalafil Acetildenafil (466) Vardenafil analogue (312)Piperidenafil( 4 5 9 ) 9 8 SibutramineDesmethylsibutramine (265)98 98 43 265 1. 2. Sildenafil TadalafilVardenafilSibutramine (72~98) 1991 () 1995
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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 2009. 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