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1 3 6 Vol. 3 No Journal of Food Safety and Quality Dec., 2012 * 李萍, 杨金易, 张燕, 曾道平, 孙远明 (,,, ) 摘要 : 5,,,, 关键词 : ; ; Research progress on detection of sildenafil in health care food LI Ping, YANG Jin-Yi, ZHANG Yan, ZENG Dao-Ping, SUN Yuan-Ming * (Guangdong Provincial Key Laboratory of Food Quality and Safety, Laboratory of Quality and Safety Risk Assessment in Agricultural Products Preservation of the Ministry of Agriculture, College of Food Science, South China Agriculture University, Guangzhou , China) ABSTRACT: Sildenafil citrate is now illegally used in some health care foods as a specific phosphodiesterase type 5 (PDE) inhibitor. Because of its side effects and abuse in drug market, the detection of sildenafil in such foods has become a focus. The detection methods of sildenafil that have been reported basically include spectrophotometry, chromatography, spectrometry, capillary electrophoresis and immunoassay methods. Each method has its own advantages and disadvantages. Herein we present a summary of the research progress on detection of sildenafil in health care food. KEY WORDS: sildenafil; detection; health care food (sildenafil citrate) [1],, (cgmp) 5 (PDE5), (, Viagra) cgmp,, (ED) [2-3],, [4],,,,,, 1 分光光度法, [5-6] 基金项目 : ( ) ( ) (2010A ) (2010A ) (2011A ) * 通讯作者 :,,, : ymsun@scau.edu.cn

2 706 3 Dinesh [7] A 415 nm, 1.25~25 μg/ml (r=0.9992), 0.16 μg/ml B 460 nm, 1.5~60 μg/ml (r=0.9996), 0.18 μg/ml [8],,,, 620 nm, 0~ mol/l, ε L mol 1 cm 1, mol/l 520 nm, 0.2~ mol/l, ε L mol 1 cm 1, mol/l,,,,,,, 2 色谱技术,, [9] 2.1 薄层色谱法 (TLC), 1979 Armstrong,,, [10-11] [12],,,,,,,, 10 TLC,,,,,, 2.2 高压液相色谱法 (HPLC), [13-14] Daraghmeh [15], C 18 (3.9 mm 300 mm, 10 μm), 0.2 mol/l : (1: 1), 1 ml/min, 240 nm 2~17 μg/ml, 100.4% HPLC,,,, 2.3 液相色谱 - 质谱联用技术 (LC-MS) (LC-MS),,,,, [16] [17] - (LC-MS/ MS), C 18 (2.1 mm 100 mm, 3.5 μm), 0.01 mol/l, : : (55: 10: 35), 0.2 ml/min ESI Full Scan, SIR, Daughter 1~5 μg/ml, 103%, 105%, 98% SN/T / [5],,, 1.0 μg/mg, 0.01 μg/ml,,

3 6, : 光谱法 3.1 近红外光谱法 (NIR),, [18-19] [20],,,,,,,, 3.2 核磁共振 (NMR),,, [21-22] Wawer [23] 1 H, 13 C, 15 N,, 13 C NMR, 4 毛细管电泳 (CE) (capillary electrophoresis, CE), [24] Qin [25] -, UK-103, 320(UK) 14 min, UK 14 ng/ml 17 ng/ml, 50~600 ng/ml 40~400 ng/ml,,, -, 5 免疫分析法 [26],,, PCR, [27,28] Song [29],,, IC 50 6±0.1 ng/ml, 0.6± 0.02 ng/ml, 70%~120%,, PBS 10,, 6 结束语, ;

4 708 3, 0.16 μg/ml, ; HPLC-MS-MS CE 0.01 μg/ml μg/ml,,, ; HPLC,,,,,,, 0.6±0.02 ng/ml, 参考文献 [1]. ( )[S]. 2002: 9. [2] Behr-Roussel D, Oudot A, Caisey S, et al. Daily treatment with sildenafil reverses endothelial dysfunction and oxidative stress in an animal model of insulin resistance [J]. Eur Urol, 2008, (6): [3] Fleshner N, Harvey M, Adomat H, et al. Evidence for contamination of herbal erectile dysfunction products with phosphodiesterase type-5 inhibitors [J]. Urology, 2005, 174(2): 636. [4] McCulley TJ, Luu JK, Marmor MF, et al. Effects of sildenafil citrate (Viagra) on choroidal congestion [J]. Ophthalmologica, 2002, 216 (6): [5] Vidya Sagar G, Sastry BS, Gangadhara Rao NVS. Spectrophotometry methods of the determination of sildenafil in tablets [J]. Chem Sci, 2003, 1(3): [6],,. [J]., 2004, 20(3): [7] Dinesh ND, Nagaraja P, Made Gowda NM, et al. Extractive spectrophotometric methods for the assay of sildenafil citrate (Viagra) in pure form and in pharmaceutical formulations [J]. Talanta, 2002, 57, [8],. [J]., 2004, 20(2): [9],. [J]., 2011, 15(10): [10] Kaale E, Risha P, Layloff T. TLC for pharmaceutical analysis in resource limited countries [J]. J Chromatogr A, 2010, 1218: [11]. [J]., 2008, 12(9): [12],. [J]., 2008, 28(8): [13] Zou P, Oh SSY, Hou P, et al. Simultaneous determination of synthetic phosphor-diesterase-5 inhibitors found in a dietary supplement and pre-mixed bulk powders for dietary supplements using high-performance liquid chromatography with diode array detection and liquid chromatography [J]. J Chromatogr A, 2006, 1104(1 2): 113. [14] Guermouche MH, Bensalah K. Solid phase extraction and liquid chromatographic determination of sildenafil and N-demethyl sidenafil in rat serum with basic mobile phase [J]. J Pharm Biomed Anal, 2006, 40(4): 952. [15] Daraghmeh N, Al-Omari M, Badwan AA, et al. Determination of sildenafil citrate and related substances in the commercial products and tablet dosage form using HPLC [J]. J Pharm Biomed Anal, 2001, 25, [16] Kim J, Ji HY, Kim SJ, et al. Simultaneous determination of sildenafil and its active metabolite UK-103, 320 in human plasma using liquid chromatography/tandem mass spectrometry [J]. J Pharm Biomed Anal, 2003, 32(2): 317. [17],,. - [J]., 2010, (9): [18] Chu XL, Xu YP, Lu WZ. Research and application progress of chemometrics methods in near infrared spectroscopic analysis [J]. Chin J Anal Chem, 2008, 36(5): [19] Luypaert J, Massart DL, Vander-Heyden Y. Near-infrared spectroscopy applications in pharmaceutical analysis [J]. Talanta, 2007, 72(3): [20],. [J]., 2009, 37(12): [21] Lianga YZ, Xieb P, Chanc K. Quality control of herbal medicines [J]. J Chromatogr B, 2004, 812: [22]. [D]., [23] Wawer I, Pisklak M. 1 H, 13 C, 15 N NMR analysis of sildenafil base and citrate (Viagra) in solution, solid state and pharmaceutical dosage forms [J]. J Pharm Biomed Anal, 2005, 38: [24] Hoff R, Kist TB. Analysis of sulfonamides by capillary electrophoresis [J]. J Sep Sci, 2009, 32(5):

5 6, : 709 [25] Qin WD, Li SFY. An ionic liquid coating for determination of sildenafil and UK-103,320 in human serum by capillary zone electrophoresis-ion trap mass spectrometry [J]. Electrophoresis, 2002, 23, [26],. [M]. :, [27],. [J]., 2011, 46(2): adulterated functional foods [J]. Food Agr Immunol, 2011: ( 责任编辑 : 张宏梁 ) 作者简介李萍,, : sweetgirl1216@163.com [28] Jeon M, Paeng IR. Quantitative detection of tetracycline residues in honey by a simple sensitive immunoassay [J]. Anal Chim Acta, 2008, 626 (2): 180. [29] Song Y, Wang YY, Zhang Y, et al. Development of enzyme-linked assay for rapid determination of sildenafil in 孙远明,,, : ymsun@scau. edu.cn

Microsoft Word 熊波-二校

Microsoft Word 熊波-二校 6 3 Vol. 6 o. 3 2015 3 Journal of Food Safety and Quality Mar., 2015 * 熊波, 吴胜泽, 苏焕斌, 张燕, 刘辉 (, 528300) 摘要 : 目的 (sildenafil, SD) 方法 (SDH) (SDH-BSA),, SD, 结果 SD, 3.8 10 5, 0.02~3.8 ng/ml,, 结论 SD, SD 关键词