ality control of botanicals and botanical health products screening for adulterants and metabolomic investigations

QUALITY CONTROL OF BOTANICALS AND BOTANICAL HEALTH PRODUCTS: SCREENING FOR ADULTERANTS AND METABOLOMIC INVESTIGATIONS LI LIN NATIONAL UNIVERSITY OF SINGAPORE 2011     QUALITY CONTROL OF BOTANICALS AND BOTANICAL HEALTH PRODUCTS: SCREENING FOR ADULTERANTS AND METABOLOMIC INVESTIGATIONS LI LIN (B.Sc., XJTU) A THESIS SUBMITTED FOR THE DEGREE OF DOCTOR OF PHILOSOPHY DEPARTMENT OF PHARMACY NATIONAL UNIVERSITY OF SINGAPORE 2011     Dedicated to my parents and Vivi       ACKNOWLEDGEMENTS First of all, I would like to express my deepest and most sincere gratitude to my supervisor Associate Professor Koh Hwee Ling and co-supervisor Professor Bosco Chen Bloodworth, for their invaluable guidance, patience and kind supervision. Being their PhD student has been one of the most fortunate moments in my life. In addition, I would also like to thank Ms Low Min Yong and Dr Ge Xiao Wei from Health Sciences Authority of Singapore for their extremely generous support and valuable suggestions. The Department of Pharmacy, NUS and the Health Sciences Authority of Singapore also deserve very special thanks for the financial support (NUS graduate research scholarship) and research facilities that make this study possible. I would specially like to thank Associate Professor Chan Sui Yung, Head of the Department of Pharmacy, for her understanding and concern during my PhD study. I would like to also thank the following people whom I had worked with quite closely in NUS and in the Pharmaceutical laboratory of HSA: Dr Toh Ding Fung, Dr Hou Peiling, Mr Ching Jianhong, Ms Chay Lai Fong, Ms Teo Hong Gek Jessie, Ms Chin Lee Cheng Agnes, Dr Tan Jing, Mr Patel Dhavalkumar Narendrabhai, Dr Sogand Zareisedehizadeh, for their friendship and support. The undergraduate students who had worked with me in these labs, Miss Fransiska Aliwarga and Miss Ng Ke Ting Chelsea, also deserve big thanks for their curiosities that stimulated ideas in my research work, as well as for their helping hands. Last but not least, I would like to express my most sincere appreciation to my family for their love, continuous support during this PhD study.     I LIST OF PUBLICATIONS 1. Li Lin, Low Min-Yong, Aliwarga Fransiska, Teo Jessie, Ge Xiao-Wei, Zeng Yun, Bloodworth Bosco Chen, Koh Hwee-Ling. Isolation and identification of hydroxythiohomosildenafil in herbal dietary supplements sold as sexual performance enhancement products. Food Addit. Contam., 2009, 26(2), 145-151. 2. Li Lin, Low Min-Yong, Ge Xiao-Wei, Bloodworth Bosco Chen, Koh Hwee-Ling. Isolation and structural elucidation of dapoxetine as an adulterant in a health supplement used for sexual performance enhancement. J Pharm. Biomed. Anal., 2009, 50(5), 724-728. 3. Ge Xiaowei, Li Lin, Koh Hwee-Ling, Low Min-Yong. Identification of a new sildenafil analogue in a health supplement. 2011, 56(3), 491-496. 4. Tan Jing, Li Lin, Zeng Yun, Ge Xiaowei, Low Min-Yong. Characterization of Chinese Medicines by Comprehensive Two-Dimensional Gas Chromatography and Time-of-Flight Mass Spectrometry (GC×GC-TOFMS) with Assistance of Multivariate Data Analyses. Sep. Sci., 2011, 3(2), 5-7. 5. Low Min-Yong, Zeng Yun, Li Lin, Ge Xiao-Wei, Lee Ruth, Bloodworth Bosco Chen, Koh Hwee-Ling. Safety and quality assessment of 175 illegal sexual enhancement products seized in Red-Light districts in Singapore. Drug Saf., 2009, 32(12), 1-6. 6. Ge Xiao-Wei, Low Min-Yong, Zou Peng, Li Lin, Yin Sharon Oh Sze, Bloodworth Bosco Chen, Koh Hwee-Ling. Structural elucidation of a PDE-5 inhibitor detected as an adulterant in a health supplement. J Pharm. Biomed. Anal., 2008, 48(4), 10701075.  II 7. Low Min-Yong, Li Lin, Ge Xiao-Wei, Kee Chee-Leong, Koh Hwee-Ling. Isolation and structural elucidation of Flibanserin as an adulterant in a health supplement used for female sexual performance enhancement. J Pharm. Biomed. Anal., Accepted. 8. Li Lin, Low Min-Yong, Ge Xiao-Wei, Bloodworth Bosco Chen, Koh Hwee-Ling. Isolation and structural elucidation of a new sildenafil analogue from a functional coffee. J Agric. Food Chem., Submitted. 9. Li Lin, Low Min-Yong, Ge Xiao-Wei, Bloodworth Bosco Chen, Koh Hwee-Ling. Simultaneous determination of 19 phosphodiesterase type-5 inhibitors and analogues as adulterants in health supplements for sexual performance enhancement by high performance liquid chromatography-diode array detector. J Chromatogr. A, Submitted. 10. Li Lin, Low Min-Yong, Ge Xiao-Wei, Bloodworth Bosco Chen, Koh Hwee-Ling. A Liquid Chromatography-Linear Ion Trap-Orbitrap XL hybrid Fourier Transform Mass Spectrometry method used for characterizing the variation of Panax notoginseng extracted with different pressurized liquid extraction procedures. J Phytochem. Anal., In preparation. 11. Li Lin, Low Min-Yong, Ge Xiao-Wei, Bloodworth Bosco Chen, Koh Hwee-Ling. Metabolomic investigation of adaptogenic botanicals together with raw and steamed Panax notoginseng using non-targeted metabolite profiling coupled with multivariate data analysis approach. J Phytochem. Anal., In preparation.     III LIST OF POSTER PRESENTATIONS 1. Li Lin, Low Min-Yong, Ge Xiao-Wei, Bloodworth Bosco Chen, Koh Hwee-Ling. Metabolomic profiling of three Panax species using pressurized liquid extraction and LC-LTQ-Orbitrap XL FTMS. Poster presentation, Recent Development in Chinese Herbal Medicine Conference, 25-26 Jan 2010, Nanyang Technological University, Singapore (Best poster award). 2. Li Lin, Low Min-Yong, Aliwarga Fransiska, Teo Jessie, Ge Xiao-Wei, Zeng Yun, Bloodworth Bosco Chen, Koh Hwee-Ling. Identification of a sildenafil analogue in an internet health supplement. 22nd Federation of Asian Pharmaceutical Association Congress (FAPA 2008), 7-10 Nov 2008, Grand Copthorne Waterfront Hotel, Singapore. 3. Li Lin, Low Min-Yong, Ge Xiao-Wei, Bloodworth Bosco Chen, Koh Hwee-Ling. Metabolomic profiling of three Panax species using pressurized liquid extraction and LC-LTQ-Orbitrap XL FT MS. Poster presentation, Educating Pharmacists (Asia) Symposium, 15-16 Apr 2010, National University of Singapore, Singapore. 4. Li Lin, Low Min-Yong, Ge Xiao-Wei, Bloodworth Bosco Chen, Koh Hwee-Ling. Metabolomic profiling of three Panax species using pressurized liquid extraction and LC-LTQ-Orbitrap XL FTMS. Poster presentation, 6th AAPS-NUS Student Chapter (ANSC) Scientific Symposium, Apr 2010, National University of Singapore, Singapore. 5. Ng Chelsea, Li Lin, Ge Xiao-Wei, Low Min-Yong, Koh Hwee-Ling. Authentication of herbs by plants metabolomics. 5th AAPS-NUS Student Chapter (ANSC) Scientific Symposium, Apr 2009, National University of Singapore, Singapore.  IV 6. Aliwarga Fransiska, Ching Jianhong, Li Lin, Low Min-Yong, Koh Hwee-Ling. Screening of sexual performance enhancement and slimming products available fron the Internet for undeclared drugs. 4th AAPS-NUS Student Chapter (ANSC) Scientific Symposium, Apr 2008, National University of Singapore, Singapore.     V TABLE OF CONTENTS ACKNOWLEDGEMENTS LIST OF PUBLICATIONS LIST OF POSTER PRESENTATIONS TABLE OF CONTENTS SUMMARY LIST OF TABLES LIST OF FIGURES LIST OF ABBREVIATIONS AND SYMBOLS I II IV VI IX XII XIV XVII CHAPTER INTRODUCTION 1.1 Quality of botanicals and botanical health products 1.1.1 Factors affecting the quality 1.1.2 Methods and techniques used for quality control 1.2 Targeted adulterant screening in botanical health products 16 1.2.1 Sexual performance enhancement products 17 1.2.2 Slimming products 26 1.3 Metabolomic investigations for the quality control of botanicals 29 1.3.1 Selected botanicals for investigation 31 1.3.2 Sample extraction techniques 35 1.3.3 Metabolite fingerprinting 35 1.3.4 Data pre-processing 37 1.3.5 Multivariate data analysis 38 CHAPTER HYPOTHESES AND OBJECTIVES 40 2.1 Hypotheses 40 2.2 Objectives 40 CHAPTER TARGETED ADULTERANT SCREENING IN BOTANICAL HEALTH PRODUCTS USED FOR SEXUAL PERFORMANCE ENHANCEMENT AND SLIMMING 3.1 HPLC-DAD method development 3.1.1 Introduction  VI 42 42 42 3.1.2 Objective 44 3.1.3 Experimental 44 3.1.4 Results and discussion 48 3.1.5 Conclusion 54 3.2 Targeted adulterant screening in botanical health products used for sexual performance enhancement and slimming bought on-line 55 3.2.1 Introduction 55 3.2.2 Objectives 55 3.2.3 Experimental 55 3.2.4 Results and discussion 60 3.2.5 Conclusion 68 CHAPTER ISOLATION, PURIFICATION AND STRUCTURAL ELUCIDATION OF NEW ADULTERANTS FROM BOTANICAL HEALTH PRODUCTS USED FOR SEXUAL PERFORMANCE ENHANCEMENT 4.1 Isolation and identification of compound X 69 69 4.1.1 Introduction 69 4.1.2 Objective 70 4.1.3 Experimental 70 4.1.4 Results and discussion 73 4.1.5 Conclusion 79 4.2 Isolation and structural elucidation of compound Y 80 4.2.1 Introduction 80 4.2.2 Objective 80 4.2.3 Experimental 81 4.2.4 Results and discussion 85 4.2.5 Conclusion 93 4.3 Isolation and structural elucidation of compound Z 94 4.3.1 Introduction 94 4.3.2 Objective 95 4.3.3 Experimental 95 4.3.4 Results and discussion 98 4.3.5 Conclusion 105     VII   notoginseng. 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Eur J Mass Spectrom 13 (3): 233-238.     201   Appendices  202   Appendix 1: List of sexual performance enhancement botanical health products purchased, dosage form, quantity per package and websites. Product name Dosage form Quantity/ Package Stamina-Rx For Men Tablet 60 Stamazide Tablet 60 Cerniplex Tablet 30 Tablet 180 Capsule 60 No. Website of purchase Arginmax for Women Kohinoor Gold Maxidus for Men Capsule 20 Maxidus for Men (oil) Liquid 60 ml LFW Capsule 20 Libidus Capsule 20 10 Semenax Capsule 90 http://www.aragonproducts.com/theproducts.cf m?master=5455 http://www.aragonproducts.com/theproducts.cf m?master=6126 http://www.aragonproducts.com/theproducts.cf m?master=5999 http://www.aragonproducts.com/theproducts.cf m?master=476 http://www.ayurvediccure.com/kohinoor.htm https://www.biogulfstore.com/orders/Affiliate/ products.php https://www.biogulfstore.com/orders/Affiliate/ products.php https://www.biogulfstore.com/orders/Affiliate/ products.php https://www.biogulfstore.com/orders/Affiliate/ products.php http://www.bettersexsupplements.com/ 11 Provestra Caplet 30 http://www.bettersexsupplements.com/ 12 Viverex for Men Tablet 10 http://www.erectingconfidence.com/male_sexual_enhancement.html 13 Veromax Natural Tablet 60 14 NSI Women's Passion Booster Capsule 120 15 Max International Testosterone Herbal Capsule 60 Capsule 60 17 NSI Male Enhancement Provigro Capsule 24 18 LJ 100 Tongkat Ali Capsule 90 19 LJ 100 Freeze Dried Eurycoma Longifolia Powder 10 g 20 Testo Jack Capsule 60 21 Erox Capsule 60 22 Source Naturals, Tongkat Ali Tablet 60 23 Women RA Tablet 20 24 Slevotra Tablet 25 Vitro Man Power Plus Capsule 60 26 Virilar Capsule 30 27 XP Tongkat Ali Capsule 28 Maintain 400mg Tongkat Ali Capsule 60 16 http://www.vitacost.com/VeromaxForMenSexu alPerformanceEnhancer http://www.vitacost.com/NSI-WomensPassion-Booster-All-Natural-Extracts http://www.vitacost.com/MaximumInternational-Testosterole-Maximum-LibidoComplex http://www.vitacost.com/NSI-MaleEnhancement-Formula-with-MacaPure http://www.harvesthealth.com/provigro.html http://www.iherb.com/ProductDetails.aspx?c=1 &pid=3666&at=0 http://www.iherb.com/ProductDetails.aspx?c=1 &pid=8307&at=0 http://www.iherb.com/ProductDetails.aspx?c=1 &pid=5026&at=0 http://www.iherb.com/ProductDetails.aspx?c=1 &pid=4609&at=0 http://www.iherb.com/ProductDetails.aspx?c=1 &pid=1504&at=0 http://www.scillausa.com/womenrasildenafil.html http://www.scillausa.com/slevotravardenafil.html http://www.sexpo.com.sg/onlinestore/index.ph p?act=viewProd&productId=200 http://www.sexpo.com.sg/onlinestore/index.php?act =viewProd&productId=123507 http://www.sexpo.com.sg/onlinestore/index.php?act =viewProd&productId=123589 http://www.sexpo.com.sg/onlinestore/index.php?act =viewProd&productId=123537     203   http://www.extenzedirect.com/?a=emoshe&t=Google-INTL&c=0 http://www.paramountsupplements.com/e60camaenpi.html http://www.paramountsupplements.com/enhance9.html http://www.paramountsupplements.com/maxvirxmaen6.html http://www.paramountsupplements.com/koasseonhost.html http://www.paramountsupplements.com/liplsebo.html http://www.paramountsupplements.com/maxst30camas.html http://www.paramountsupplements.com/plpi30co.html http://www.paramountsupplements.com/proplpi60cap.html http://www.paramountsupplements.com/riformen10ca.html http://www.paramountsupplements.com/ri212cabo.html http://www.paramountsupplements.com/rxerect.html http://www.paramountsupplements.com/stimuloid.html http://www.paramountsupplements.com/vimaenfo.html http://www.paramountsupplements.com/viacil30ct.html http://whttp://www.vigorexonline.com/ http://www.enaturalremedies.com/ikawe_for_s exual_performance.htm http://www.enaturalremedies.com/thanda_for_ passion_libido_boosting.htm 29 Extenze Capsule 60 30 E-Long-Ate Capsule 60 31 Enhance-9 Tablet 30 32 Max Vitality Rx Capsule 60 33 Kong Herbal Enhancer Tablet 60 34 Liquid Rx Liquid 30 ml 35 Max Stamina Capsule 30 36 Pleasure Pills Capsule 30 37 Pro Plus Pills Tablet 60 38 Rigid for Men Capsule 10 39 Rize-2 Capsule 12 40 Rx Erect Capsule 30 41 Stimuloid Capsule 30 42 Vialafil Capsule 30 43 Viacil Tablet 30 44 Vigor-Ex Capsule 45 Ikawe Liquid 50 ml 46 Thanda Capsule 60 47 Pro-Solution Pills Tablet 60 http://www.prosolutionpills.com/?a=101858&c=0 48 VigRx Capsule 60 49 Bali Mojo Capsule 10 http://www.vigrx.com/?a=nudei096&c=0 http://www.balimojo.com/?gclid=CLPu66urm4 4CFR3JYAod7xk1TQ http://www.vitroman.com/en/index_en.asp?pag eID=tongkat-ali-100 http://www.vitadigest.com/erexin.html Capsule 60 51 Vitro Man Tongkat Ali 100 Erexin Tablet 90 52 Avela Capsule 30 53 Vivid Virility Tablet 72 54 Virility Ex Pills Tablet 60 55 Kama Raja Capsule 60 http://www.kamaraja.com/index.htm?aff=google1 56 Vimax Better Man (Light brown) Better Man (Dark brown) Capsule 30 Capsule 40 Capsule 40 59 Marathon 21 Tablet 60 60 Alpha Male Plus Capsule 60 http://www.pillsexpert.com/penispills/ http://www.wholesalesupplementstore.com/bett erman.html http://www.wholesalesupplementstore.com/bett erman.html http://www.lhslive.com/product_info.php?prod ucts_id=113 http://www.lhslive.com/product_info.php?prod ucts_id=108 50 57 58  204 http://www.vitadigest.com/avela.html http://www.vitadigest.com/vivid-virilitymen.html http://www.ultraherbal.com/product/overview/ Virility_Pills_For_Men/   61 Zenerx Capsule 60 http://www.zenerx.com/ 62 H-Force Capsule 60 http://www.vitavips.com/studmax.php 63 Provigrax Tablet 60 http://www.vitavips.com/provigrax.php 64 MX MAN Capsule 60 65 Vaxitrol Capsule 16 66 Stamitrol Tablet 30 67 Xiadafil Tablet 68 XOMAX Capsule 30 http://www.vitavips.com/mx-man.php http://www.paramountsupplements.com/vaxitrol.html http://www.paramountsupplements.com/stamitrol30ct.html http://www.paramountsupplements.com/xiadafil.html http://www.xomax-man.com/ 69 Erotica Plus Capsule 60 https://www.buyxomax.com/products.php?pg=2 70 Yang Pro Tablet 60 https://www.buyxomax.com/products.php?cat=1 71 Sex Pill Capsule 60 https://www.buyxomax.com/products.php?cat=1 72 Capsule 60 Powder 240 g Powder 240 g 75 Sure-Erect SAS LABS - Sexual Health Package ESE LABS - Sexual Health Package YERBA - DIET Capsule 30 76 Cravex Capsule 90 77 Lean Tabs Tablet 90 78 Oyama-Rectic Capsule 30 79 Super Citrimax Capsule 90 80 Lyse XL SZM Formula for Men Capsule 90 Capsule 10 82 Mega V Capsule 10 83 Perfomaxxx Herbal Sex Pills Capsule 10 http://www.mensexpills.net/sureerect.php http://www.internationalsupplements.com/prod uct_info.php?products_id=234 http://www.global-supplements.com/SexualHealth-Package/ http://www.vitavips.com/yerbaslim.php http://www.vitadigest.com/natrol-cravex90.html http://www.vitadigest.com/lean-tabs.html http://www.vitadigest.com/dyma-reticdymatize.html http://www.nutrasanus.com/super-citrimaxproduct.html http://www.vitavips.com/lyse-xl.php http://www.netpharmacy.co.nz/szm-formulafor-men-1 http://www.netpharmacy.co.nz/65/group/85/pa ge/1/style/megav10c/Mega+V+Herbal+Enhanc ement+500mg+10+Caps http://www.netpharmacy.co.nz/65/group/85/pa ge/1/style/perforMaxx10p/Performaxx+Herbal +Sex+Pill+10+Caps 84 Avaprex Capsule 60 85 In Control Capsule 60 86 Reveal Tablet 60 87 TestoraNx Tablet 60 http://www.wholesalesupplementstore.com/fatattack-stack.html http://www.wholesalesupplementstore.com/fatattack-stack.html http://allnutri.com/pid38657/testoranx.aspx 88 Horny Goat Weed Capsule 30 http://www.evitamins.com/product.asp?pid=10424 89 Rizer XL Capsule 60 90 Tribuloid Capsule 60 91 Damiana leaves Capsule 100 92 Moodmax Tablet 60 93 Natural V for Men Capsule 60 94 Viraloid Capsule 60 http://www.rizerxl.com/ http://www.herballoveshop.com/product.asp?PI D=14351 http://www.herballoveshop.com/product.asp?PI D=1564 http://www.herballoveshop.com/product.asp?PI D=1007 http://wholesalesupplementstore.com/naturalvformen.html http://www.herballoveshop.com/product.asp?PI D=18367 73 74 81 http://www.avaprex.com/adipex.htm?gclid=COmk4 KOB344CFQEgYAodCWILSg     205   95 Excite Capsule 90 http://www.evitamins.com/product.asp?pid=5654 96 Aziffa Capsule http://supplementkingdom.com/azzifa.html 97 Vigralis Capsule 12 98 MacaActive Tablet 100 99 Elexia Plus Tablet 60 100 Tigra Men Tablet 56 101 Blue Up Capsule 60 http://supplementkingdom.com/v_gralis.html http://www.natural-male-health.com/ordermacaactive.htm http://www.vitadigest.com/elexia-men.html http://www.body4real.co.uk/product.php?produ ctid=17948 http://supplementkingdom.com/blue_up.html 102 Hypertest Capsule 120 103 Nature's way Horny Goat Weed Capsule 60 104 Paravol Male Enhancer Capsule 60 105 Sida Cordifoloia Capsule 40 106 Hot Rod Capsule 10 107 Libido & Drive 108 109 110 111 Performance & Stamina Horny Goat Weed Extract (Healthy direct) Deer Antler Plus Maxine's Intima for women http://supplementkingdom.com/hypertest.html http://shopping.yahoo.com/p:Nature%27s%20 Way%2C%20Horny%20Goat%20Weed%2C% 20%2860%20Capsules%29:2002637149;_ylt= AkH7oFIxbtShBHY3AHEzzcPWyMUu http://www.evitamins.com/product.asp?pid=6289 Tablet 90 Capsule 60 http://www.expresschemist.co.uk/Sida_Cordifo lia_by_Reflex.html http://www.amazon.com/dp/B000WACYCU?s mid=A3AC8PQ96D2D8O&tag=shopzilla_rev_ 1271-20&linkCode=asn http://www.iherb.com/ProductDetails.aspx?c=1 &pid=3147&at=0 http://www.iherb.com/ProductDetails.aspx?c=1 &pid=3147&at=0 http://www.healthydirect.com/product/HNYG W/d.jsf http://www.deerantlerplus.com/ Tablet 60 http://www.evitamins.com/product.asp?pid=199 Liquid soft-gel Liquid soft-gel 60 60 112 Sexy Lady Capsule 60 http://www.evitamins.com/product.asp?pid=7301 113 Adios Max Tablet 60 http://www.expresschemist.co.uk/AdiosMax.html Tablet 60 http://www.evitamins.com/product.asp?pid=10424 Capsule 30 http://www.evitamins.com/product.asp?pid=6438 Capsule 60 http://www.evitamins.com/product.asp?pid=6437 Tablet 120 http://www.evitamins.com/product.asp?pid=1374 117 Horny Goat Weed (Epimedium) RedHorn KONG Black Voodoo Male Power 118 Semenax Tablet 20 119 Cockstar Capsule 14 http://www.bettersexmall.com/semenax_review .html?ss=e0585fe84e49c5973a59de11a1e7ce87 http://www.vitadigest.com/cockstar.html 120 24/7 Sure XP Tongkat Ali for Men Supreme Capsules Capsule 60 http://www.strictlyhealth.com/viagra_alternative.php Capsule 40 http://www.sexpo.com.sg/onlinestore/index.php?act =viewProd&productId=123589 Avlimil Capsule 30 http://www.aragonproducts.com/theproducts.cf m?master=5936&owner=694 Capsule 60 Capsule 60 Capsule 30 114 115 116 121 122 123 124 125  206 Ejaculoid Semen Volumizer Spermamax Male Virility Sex Cycle http://www.aragonproducts.com/theproducts.cfm?cat =1&master=6830&owner=694&subcat=578 http://www.aragonproducts.com/theproducts.cfm?cat =1&master=6436&owner=694&subcat=578 http://www.aragonproducts.com/theproducts.cf m?cat=1&master=7553&owner=694&subcat= 2114   126 Manhood Max Capsule 60 127 SutraMax Capsule 128 Cobra Capsule 60 129 AriZe Capsule 10 130 Ball Refill Capsule 30 131 Sustanol Tablet 30 132 Orexis Capsule 60 133 Expand capsules Capsule 60 http://www.aragonproducts.com/theproducts.cf m?cat=1&master=8151&owner=694&subcat= 2114 http://www.aragonproducts.com/theproducts.cf m?cat=1&master=8987&owner=694&subcat= 2114 http://www.aragonproducts.com/theproducts.cf m?cat=1&master=8768&owner=694&subcat= 2114 http://www.aragonproducts.com/theproducts.cf m?cat=1&master=9280&owner=694&subcat= 2114 http://www.aragonproducts.com/theproducts.cf m?cat=1&master=9813&owner=694&subcat= 2114 www.aragonproducts.com/theproducts.cfm?ma ster=6258 http://www.aragonproducts.com/theproducts.cf m?master=6030 http://www.expandcapsules.com/ 134 King Cobra Capsule 40 http://favstore.net/kingcobra/order.php 135 Roaring tiger Capsule 28 http://www.roaringtiger.com/free_trial_offer.php 136 ErogenX Capsule 60 http://www.intimatewholesalers.com/a83089.html 137 Vicerex Capsule 10 http://www.aragonproducts.com/theproducts.cfm?cat =0&master=7435&owner=694&subcat=0 138 Sizepro Ultra Tablet 30 http://www.ordersizepro.com/?hostid=bettersex mall.com&src=bettersexmall.com 139 Performax Ultra all Natural Male Performance Enhancer Tablet 60 http://www.wellnessalternatives.com/cart/?prod uct=WAPERMX01 140 Mxman Capsule 60 141 Virility Pills Capsule 60 142 Katana Tablet 60 http://www.bettersexmall.com/katana_review.html 143 Last longer Tablet 60 144 Gokshura Capsule 60 145 Virile Tablet 50 146 Stinger Rx Capsule 30 147 Man's Favorite Capsule 10 http://www.mensexpills.net/lastlonger.php http://www.ayurvediccure.com/tribulusterrestris.htm http://www.vitasprings.com/virile-onebiotech.html http://www.vitasprings.com/stinger-rx--1-maleenhancement-formula.html http://www.vitasprings.com/man-s-favorite-farlong.html 148 Herbal virility Tablet 90 149 Herbal V Capsule 10 150 AlcoholX Capsule 151 Mr Energy Capsule 152 Azikiwe plus Tablet 60 153 Volume Pills Tablet 60 http://www.mxman-herbal-penis-enlargementpills.com/ordernow.php http://www.buyvprx.com/?hostid=bettersexmal l.com&src=bettersexmall.com http://www.vitasprings.com/herbal-virilitymale-performance.html http://www.vitasprings.com/herbal-v-10-capslane-labs.html http://www.alcohol-x.com/ http://www.mrenergypills.com/order.html http://www.azikiweplus.com/?hostid=bettersex mall.com&src=bettersexmall.com http://www.aragonproducts.com/theproducts.cfm?cat =0&master=6103&owner=694&subcat=0     207   154 Erosyn for women Nokomis Tablet 30 155 MOJO Sensation Tablet 30 156 StamaLong Capsule 157 Zencore Capsule 10 158 Kapsul Tongkat Ali Hitam Plus Capsule 60 159 Kapsul Tongkat Ali Capsule 60 160 Vitality for men Capsule 60 161 Climaxol Female Sexuality Enhancement Capsule 10 162 Extenzol Capsule 20 163 Sensuvive Capsule 60 164 Venerx Capsule 60 165 BlueRise Capsule 30 Capsule 180 Bag 20 166 167 Arginmax for Women Horny Goat Weed Tea 168 Ropex Tablet 90 169 Nymphomax Capsule 60 http://www.feelgoodnatural.com/catalogue/BE LL123.html https://www.herbalsex.com/product.php?produ ctid=16162&cat=0&page= http://www.herbalsex.com/product.php?produc tid=16167&cat=318&page=1 https://www.herbalsex.com/product.php?produ ctid=16169&cat=0&page= http://cgi.ebay.com/KAPSUL-TONGKATALI-HITAM-PLUS-for-mensex_W0QQitemZ170430145827QQcmdZView ItemQQptZUK_Health_Beauty_Vitamins_Sup plements?hash=item27ae6da523 http://herba2u.net/ekedai/details/81/15/permata-hijrah/kapsultongkat-ali.html http://www.nutritionaltree.com/reviews/men/vit amins/melaleuca_vitality-for-men.aspx http://www.vitalfoodstore.com/female-libidoproduct-female-libido-booster-p/700018.htm http://www.aragonproducts.com/theproducts.cf m?master=9253 http://www.aragonproducts.com/theproducts.cf m?master=8292&owner=694 http://www.aragonproducts.com/theproducts.cf m?master=7429&owner=694 http://nitropoppers.com/bluerisefromthemakers ofnasutra.aspx http://www.americanlifestyle.com/theproducts. cfm?master=477 http://www.vitaminshoppe.com/store/en/browse/sku _detail.jsp?fromCatId=cat10411&id=TF-7034 http://www.americanlifestyle.com/theproducts. cfm?cat=1&master=6484&owner=651&subcat =128 http://www.americanlifestyle.com/theproducts. cfm?master=5551&owner=651 http://www.vitamaker.com/dr-joelenlargement-60.html http://www.vitamaker.com/enzyte.html Capsule 60 171 Dr Joel Penis Enlargement Pills Enzyte Tablet 10 172 Liquid Rise Liquid 150 ml 173 NSI Muira Puama Capsule 120 174 NSI Healthy Libido Capsule 180 175 Goliath Ejaculoid Capsule 120 176 Maxaman Capsule 60 177 XXLarge Tablet 30 http://www.vitamaker.com/liquid-rise.html http://www.vitacost.com/NSI-MuiraPuama#IngredientFacts http://www.vitacost.com/NSI-HealthyLibido#IngredientFacts http://www.vitacost.com/Goliath-LabsEjaculoid-Natural-MaleExplosions#IngredientFacts http://www.aragonproducts.com/theproducts.cf m?master=5557&owner=694 http://www.vitadigest.com/xxlarge.html 178 Herbal Quiver Tablet 30 http://www.vitadigest.com/herbal-quiver.html 179 Elexia Plus Tablet 60 180 Female Sexual Tonic Liquid oz 181 Bai He Di Huang Capsule Capsule http://www.vitadigest.com/elexia-women.html http://canadiandrugshop.com/item.php?id=3430 http://www.herbsensation.net/sex-enhancerbai-he-di-huang-6-capsules-35-p.asp 170  208   http://www.herbsensation.net/sex-enhanceremperor-29-p.asp http://www.asianangel.co.uk/_shop/product_inf o.php?products_id=45 http://www.asianangel.co.uk/_shop/product_inf o.php?products_id=48 http://www.asianangel.co.uk/_shop/product_inf o.php?products_id=49 http://www.tadalissx.net/ http://www.shopwars.com/Shop/Control/Produ ct/fp/vpid/7016054/vpcsid/0/SFV/31959 http://www.provestra.com/order.html http://www.paramountsupplements.com/desire.html http://www.paramountsupplements.com/muscle-warfare-depthcharge-20-caps.html 182 Emperor Capsule 183 Fu Bao Capsule Capsule 30 184 Superdragon Capsule 185 Atlas Pills Capsule 186 Tadalis - SX Tablet 10 187 FertilAid Capsule 30 188 Provestra Tablet 30 189 Desire Capsule 190 Depth Charge Tablet 20 Tablet 10 Tablet 60 Capsule Tablet 60 Cream - Capsule 90 Tablet 30 http://www.vitadigest.com/extenze.html Capsule 10 https://www.zencore.com/ 191 192 193 194 195 196 197 198 72 Hours The Ultimate Male Enhancement Formula Dr. Boss Penis Rejuvenator Hour Sex Herbal Vivid Male Enhancement Julian's Rock Hard Cream JO System Penis Enlargement ExtenZe New & Improved Zencore Plus http://www.paramount-supplements.com/72hours-male-enhancement-formula.html http://www.paramount-supplements.com/penisrejuvenator-virility-pills.html http://www.paramountsupplements.com/sports-one-8-hour-sexsexual-pleasure-enhancer.html http://www.herbalvivid.com/indexmain.php?W MID=11407 http://www.vitamindeal.com/julian-rock-hardcrm.html http://www.systemjo.com/index.php?page=sho p.product_details&flypage=shop.flypage&prod uct_id=209&category_id=13&manufacturer_id =0&option=com_virtuemart&Itemid=26&vmc chk=1     209   Appendix 2: List of slimming botanical health products purchased, dosage form, quantity per package and websites. No. Product Name DAY FAT BURNER XTREME (7DFBX) 72 Hour Slimming Pill Dosage form Quantity/ Package Website of purchase Capsule 160 http://www.7-dfbx.com/ Capsule 60 http://www.72hourslimmingpill.com/ AmbiSlimPM Capsule 60 http://www.ambislim.com/ LipoSeduction Capsule 30 http://www.liposeduction.com/ Easiness beauty Capsule 30 http://www.drug-store-china.com/slim/treasure/ BOLDEX Capsule 60 http://www.goodnessdirect.co.uk/cgilocal/frameset/detail/925267_Potter_s_Boldex___100_ta blets.html SLIM 1-2-3 Tablet 90 http://www.cljhealth.com/weight_loss.htm Slim-Rite Tablet 90 FITANSLIM Powder 150 g 10 Slimthru Liquid 7.5 ml Bag 10 http://www.9k9.com.cn/ Bag 20 http://beautytcm.com/Super%20Slimming%20Gel.html Pill 300 http://www.alibaba.com/productfree/101636387/Merit_Slimming_Pills.html Pill 300 Tablet 60 11 12 13 Slimming drinking tea Mustika Ratu Slimming Tea Merit Natural Body Slimming http://www.worldwideshoppingmall.co.uk/bodysoul/slim-rite.asp http://www.thinknatural.com/products/114422/BionalFitanslim-40s.htm http://www.expresschemist.co.uk/slimthru_weight_loss_ supplement.html http://www.alibaba.com/product/id1002193841025197610/Sinamon_Rose_Natural_beautifying_pills.html http://www.jamuramuanmadura.com/products/JAMUPELANGSING-BADAN,-Jamu-Bobot-Idaman,-ObatPenurun-Berat-Badan.html http://www.shopmania.com/shopping~online-bathbody~buy-susut-perut-super-48-pills-to-reduce-fat~p9625043.html http://www.vitaminshoppe.com/store/en/browse/sku_det ail.jsp;jsessionid=VOOLTP0FYH5UMCQUC4YFAGIK CQL00UNE?id=TF-1007 http://www.vitaminshoppe.com/store/en/browse/sku_det ail.jsp;jsessionid=VOOLTP0FYH5UMCQUC4YFAGIK CQL00UNE?id=TF-7011 14 Sinamon Rose 15 Bobot Idaman 16 Susut Perut Super Pill 48 17 Super Slimming Herbal Tea Bag 20 18 Slimming Special Tea Bag 10 Capsule 90 https://www.uniquehoodia.com/online1.php Capsule 40 http://www.ephedrasilhardcore.com/ 19 20 Unique Hoodia Ephedrasil Hardcore 21 Fenphedra Capsule 69 http://www.fenphedra.com/ 22 DecaSlim Slimming Pill Capsule 60 http://decaslim.com/ 23 Day Detox Capsule 14 http://www.7day-detox.com/  210   24 Apidexin Capsule 60 http://www.apidexin.com/ 25 Fenterdren Capsule 90 http://www.fenterdren.com/ 26 Alvitum Powder 6.45 oz http://www.americanlifestyle.com/theproducts.cfm?cat= 58&master=8375&owner=651&subcat=2069 27 Lipotea Capsule 60 http://www.lipotea.com/ 28 Anoretix Capsule 60 http://www.anoretix.com/ 29 Healthslim Capsule 90 30 Lepti-Trim Capsule 60 Capsule 60 Bag 20 Bag 20 Bag 30 Pill 200 http://www.herbsensation.net/nong-suo-jian-fei-wanslimming-pills-buy-1-get-1-free-7-p.asp Capsule 40 http://www.herbsensation.net/zhen-you-mei-weight-losscapsules-buy-2-get-1-free-8-p.asp 31 32 33 34 35 36 Acai Amazon Burn XinYan Slimming Tea Piao Yi Slimming Tea Swan slimming tea Nong Suo Jian Fei Wan Slimming Pills Zhen You Mei http://www.americanlifestyle.com/theproducts.cfm?cat= 58&master=7624&owner=651&subcat=2069 http://www.paramountsupplements.com/slfawile180c.html http://www.paramount-supplements.com/acai-amazonburn.html http://www.herbsensation.net/xinyan-slimming-tea-20tea-bags--box-15-p.asp http://www.asianangel.co.uk/_shop/product_info.php?pr oducts_id=30 http://www.herbsensation.net/swan-slimming-tea-30-teabags--box-4-p.asp 37 SoloSlim Capsule 60 http://www.soloslim.com/ 38 Aminoforce Capsule 100 http://www.newton-everett.com/category.aspx?CID=706 39 Xanthadrene Capsule 90 http://www.newton-everett.com/category.aspx?CID=706 40 Oxotrim Tablet 150 http://www.newton-everett.com/category.aspx?CID=706 41 Isotropin Sachet 30 http://www.biovea.net/product_detail.aspx?PID=1773&CID=0 Capsule 100 http://www.rain-tree.com/cha-de-bugre-capsules.htm Capsule 60 http://www.amazonslimatox.com/ Pill 90 http://www.shopwars.com/Shop/Control/Product/fp/vpid/ 5386528/vpcsid/0/SFV/31959 http://www.natural-alternative-products.co.uk/femmeslender-couture-curves-90-tablets-p-1241.html 42 43 Cha de Bugre (Cordia salicifolia) Pure Amazon Acai Slim A to X 44 Nuphedrine 45 Femme Slender Couture Curves Tablet 90 46 Caudalie Bag 30 g 47 Cheat Tabs Tablet 30 48 Blaze Capsule 60 http://www.paramount-supplements.com/blbysannu.html 49 Slimming I Capsule 30 http://www.naturallydirect.net/thyroid-weight-losspill.html http://www.beautyexpert.co.uk/Caudalie-DrainingOrganic-Herbal-Teas-30g-PRODCDTA1/ http://www.paramountsupplements.com/chta90tabyfi.html     211   50 SLIM-1 Metabo Plus Capsule 30 http://www.naturallydirect.net/weight-loss-herb.html 51 Slimming II Capsule 30 http://www.naturallydirect.net/weight-loss-detox.html 52 Pai You Su Pill 50 53 Lean System Capsule 90 54 Liposafe Capsule 60 55 Dietrine Capsule 60 56 The body-Kit Eat & Cheat Tablet 90 57 Hoodia 1000 Capsule 90 58 Zotrim Tablet 180 59 Lipobind Capsule 60 60 Metabosafe Capsule 60 61 Lipotrexate Capsule 60 62 Fat Stripper Tablet 90 63 Adios Tablet 100 64 Helix Slim Tablet 60 65 Anti Fat Tablet 90 66 Lipothin Capsule 60 67 Nutridrine Capsule 60 Capsule 120 http://www.slimquickonline.com/ Capsule 120 http://www.nutrexlipo6.com/lipo-6-ephedra-free.html 68 69 SlimQuick Hoodia Lipo Ephedra Free http://www.alibaba.com/productgs/325559585/FAN_HOU_QING_PAI_YOU_SU.html http://www.expresschemist.co.uk/product_8222_leansystem7-90-capsules.html http://www.worldwidebestsupplements.com/supplements _Liposafe_601.html http://www.worldwidebestsupplements.com/supplements _Dietrine%20Carb%20Blocker_695.html http://www.expresschemist.co.uk/product_6620_eat-andcheat.html http://www.worldwidebestsupplements.com/supplements _Hoodia%201000_582.html http://www.expresschemist.co.uk/product_3584_zotrim---2-x-90-tablets.html?newcurrency=3 http://www.expresschemist.co.uk/Lipobind-Fat-Binderx60.html http://www.worldwidebestsupplements.com/supplements _MetaboSafe_604.html http://www.worldwidebestsupplements.com/supplements _Lipotrexate_603.html http://www.expresschemist.co.uk/product_6621_fatstripper.html http://www.expresschemist.co.uk/product_3585_adios100x.html http://www.expresschemist.co.uk/product_7621_helixslim-tincture-tablets-60x.html http://www.expresschemist.co.uk/product_6619_antifat.html http://www.worldwidebestsupplements.com/supplements _LipoThin_602.html http://www.worldwidebestsupplements.com/supplements _Nutridrine%20%20Powerful%20carb%20blocker_613.html 70 Curvelle Capsule 100 http://www.wholesalesupplementstore.com/curvelle.html 71 Phase Carb blocker Capsule 60 http://www.wholesalesupplementstore.com/phase-2carb-blocker.html 72 NOXYCUT Capsule 75 http://www.noxycut.com/ 73 Youth Elixir Liquid 500 ml http://www.beautyheaven.com.au/brands/1274-Youth-Elixir  212   Appendix 3: The English and Chinese names of botanicals purchased from different sources. Source * BB EYS JL MT NICPBP SC TS TYS WS WYN English name Chinese white ginseng Korean ginseng Chinese white ginseng Korean ginseng Chinese red ginseng Chinese white ginseng Chinese red ginseng Panax notoginseng Chinese white ginseng Panax quinquefolium Panax notoginseng Chinese white ginseng Chinese red ginseng Panax quinquefolium Korean ginseng Chinese red ginseng Panax quinquefolium Panax notoginseng Panax notoginseng Chinese white ginseng Chinese red ginseng Korean ginseng Eleutherococcus senticosus Gynostemma pentaphyllum Rhodiola rosea Chinese name 中国白参 高丽参 中国人参 高丽参 吉林参 中国白参 吉林参 三七 人参 西洋参 三七 中国白参 石柱参 西洋参 高丽参 吉林参 西洋参 三七 三七 人参 吉林参 高丽参 刺五加 绞股兰 红景天 * BB : Bee’s Brand birds nest & health products Pte Ltd. (64-66 Smith Street, Singapore); EYS : Eu Yan Sang Pte Ltd. (21 Ubi Road I, Singapore); JL : Jilin province (China); MT : Ming Tai medical shop (Blk 34, Upper Cross Street, #01-150, Singapore); NICPBP : National Institute for the Control of Pharmaceutical and Biological Product (Beijing, China); SC : Sinchong Traditional Chinese Medicine (50 Temple Street, Singapore); TS : Thye Shan Medical Hall Pte Ltd. (201 New Bridge Road, Singapore); TYS : Teck Soon Medical Hall Pte Ltd. (No. 281 South Bridge Road, Singapore); WS : Wenshan (Yunnan province, China); WYN : Wong Yiu Nam Medical Hall Pte Ltd. (51 Temple Street, Singapore).       213 [...]... efficacy and safety of the botanicals and botanical health products being used Although quality control of     1   botanicals and botanical health products is challenging because of their complex nature, various methods have been developed to control their quality 1.1 Quality of botanicals and botanical health products Ensuring that botanicals and botanical health products are of suitable quality is... affecting the quality In order to control the quality of botanicals and botanical health products, it is necessary to understand the different factors which could affect the quality of botanicals  2 and botanical health products before actual quality assessment is carried out It is well established that botanicals and botanical health products quality and quality variations are due to both intrinsic and extrinsic... useful tool for the quality evaluation of these 5 adaptogenic botanicals and P notoginseng In conclusion, the work presented in this thesis has provided a new screening method for adulterants and a new metabolomic platform for evaluating the quality of  X botanicals and botanical health products The methodologies developed and applied are important to ensure the quality of health products and hence the... procurement of botanical health products used for slimming 58 Table 3.6 List of sexual performance enhancement botanical health products and compounds detected 62 Table 3.7 The concentrations of PDE-5 inhibitor and their analogues detected in 5 botanical health products 66 Table 3.8 List of slimming botanical health products and the compounds detected 67 Table 4.1 NMR data of thiohomosildenafil and compound... botanical supplements in North America highlighted the lack of quality control (Fitzloff et al., 1998) The results showed that the contents of ginsenosides of 232 Panax ginseng and 81 Panax quinquefolius products ranged from not detectable to 13.54% and 0.009% to 8.00%, respectively Hence, in order to guarantee a good and consistent quality of botanicals and botanical health products, the quality control. .. in the botanical health product samples have resulted in severe adverse reactions Screening for the presence of synthetic drugs illegally added into botanical health products is important to ensure the quality of botanical health products and to safeguard the interests and safety of consumers A new and simple HPLC-DAD method was developed, optimized and validated for the simultaneous detection and determination... active components in botanicals and botanical health products, the whole botanicals and botanical health products could be employed for evaluating their quality 1.1.2.1 Morphological, microscopic and chemical methods Conventionally, the quality control of botanicals is largely based on routine morphological identification method and microscopic identification method Physical and chemical identification... maintain well-being while botanical health products are products derived from botanicals and are usually sold over the counter as dietary supplements used for the pursuit of health and well-being (Bast et al., 2002; WHO, 1996; Liu, 2011; NCCAM, 2010) The 2007 National Health Interview Survey (NHIS) has found that 2535% of population in US uses botanicals and/ or botanical health products (Barnes et al.,... antianxiety agents or sleep aids for dealing with the stress and pressure of daily life (Cardellina, 2002) The popularity of botanicals and botanical health products is accompanied by questions regarding the quality, safety and efficacy of commercially available botanical products Quality, safety and efficacy are three interrelated issues Quality is the basic starting point and is the paramount issue because... Asian countries, such as China, Japan and Singapore The reasons individuals take botanicals and/ or botanical health products probably vary as much as people do For some person, using botanicals is part of a pattern of returning to nature, combined with eating organically grown foods and following a generally healthy diet and physically active lifestyle For others, botanicals represent a mild alternative . apply them for the quality control of botanicals and botanical health products. Firstly, for the quality control of botanical health products used for sexual performance enhancement and slimming,. QUALITY CONTROL OF BOTANICALS AND BOTANICAL HEALTH PRODUCTS: SCREENING FOR ADULTERANTS AND METABOLOMIC INVESTIGATIONS LI LIN (B.Sc., XJTU) A THESIS SUBMITTED FOR THE.   QUALITY CONTROL OF BOTANICALS AND BOTANICAL HEALTH PRODUCTS: SCREENING FOR ADULTERANTS AND METABOLOMIC INVESTIGATIONS LI LIN NATIONAL UNIVERSITY OF SINGAPORE