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1 8 5 Vol. 8 No Journal of Food Safety and Quality May., 2017 李建辉 1, 张朝晖 1*, 王琳 2, 韩深 1, 程甲 3, 何悦 1, 崔凤云 1, 赵善贞刘韦华 1, 李小林 1, 刘鑫 1, 严华 1, 齐鹤鸣 1 1, 吕东阳 (1., ; 2., ; 3., ) 3, 摘要 :,, 6, 3, -,,, -,, 关键词 : ; ; ; ; ; ; ; Research progress of analysis of illegal additives in weight-reducing dietary supplements LI Jian-Hui 1, ZHANG Zhao-Hui 1*, WANG Lin 2, HAN Shen 1, CHENG Jia 3, HE Yue 1, CUI Feng-Yun 1, ZHAO Shan-Zhen 3, LIU Wei-Hua 1, LI Xiao-Lin 1, LIU Xin 1, YAN Hua 1, QI He-Ming 1, LV Dong-Yang 1 (1. Beijing Entry-Exit Inspection and Quarantine Bureau, Inspection and Quarantine Testing Center, Beijing , China; 2. General Administration of Quality Supervision, Inspection and Quarantine of the People s Republic of China, Research Center for international inspection and Quarantine Standard and Technical Regulation, Beijing , China; 3. Shanghai Entry-Exit Inspection and Quarantine Bureau, Technical Center for Animal Plant and Food Inspection and Quarantine, Shanghai , China) ABSTRACT: After a brief introduction of the definition and risk factors of overweight and obesity, this paper presented and discussed the types, extraction and detection methods of illegal additives in weight-reducing dietary supplements. More than 100 synthetic drugs are adulterated into dietary supplements individually or in combination, including appetite suppressant, energy expenditure enhancer, drugs for preventing digestion and absorption, drugs for influencing lipid metabolism, diuretic and antidepressant. The applicability and limitations of existing analytical methods were summarized. Compared with gas chromatography, thin layer chromatography, enzyme linked 基金项目 : (2015IK IK021) Fund: Supported by Science and Technology Planning Project of General Administration of Quality Supervision, Inspection and Quarantine (AQSIQ) of P.R. China (2015IK012 and 2016IK021) * 通讯作者 :,,, [email protected] *Corresponding author: ZHANG Zhao-Hui, Ph.D, Senior Engineer, Inspection and Quarantine Testing Center, Beijing Entry-Exit Inspection and Quarantine Bureau, No.6 TianshuiyuanJie, Chaoyang District, Beijing , China. [email protected]

2 immunosorbent assay and nuclear magnetic resonance, high performance liquid chromatography combined with tandem mass spectrometric detection is the most commonly used technique. For tablets, capsules and granules, liquid solid extraction is the main sample pretreatment method. Although the current analysis methods can basically meet the actual detection requirements, there are some defects in the face of new drugs and high throughput screening, such as simultaneously extracting and pre-treating of the compounds with different polarities and improving the speed of analysis for high throughput screening. Direct analysis in real time-high resolution mass spectrometry has the advantages of high speed, accuracy and efficiency, which can be used to fill the gaps and screen illegal additives in weight-reducing dietary supplements. KEY WORDS: weight-reducing dietary supplements; illegal additive; high performance liquid chromatography; gas chromatography; thin layer chromatography; enzyme linked immunosorbent assay; mass spectrometry; nuclear magnetic resonance 1 引言,,,,,, (over the counter, OTC), ( ) [1],,,,,,,, [2] [3],,, [4],, (1), (solid-liquid extraction, SLE) - (liquid-liquid extraction, LLE) (desorption corona beam ionization, DCBI) QuEChERS(quick, easy, cheap, effective, rugged, safe) ; (2), (thin layer chromatography, TLC) (liquid chromatography, LC) (capillary electrophoresis, CE) (ion mobility spectrometry, IMS) (gas chromatography, GC) X (X-ray diffraction, XRD) (enzyme-linked immunosorbent assay, ELISA) (nuclear magnetic resonance, NMR), 2 非法添加物种类 [2-64], 111 ( 1), [5-7], : (1) ( N- N- ); (2) ( β- ); (3) ( ); (4) ( ); (5) ( ); (6) ( ) 3 检测方法 [2,4,5,7-58], (diode array detector, DAD) [4,31,42,50] (fluorescence detector, FLD) [8,13] (mass spectrometer, MS) [4,24,27,29,30,35,36,40,41,43,44,49,51-55], [4,8,40,54] [12,56] (attenuated total reflectance infrared spectroscopy, ATR-IR) [57] [16] - [3] X [58] [59]

3 5, : 1587 表 种违法添加化合物信息表 Table 1 Information of 111 illegal additives CAS 1 althiazide C 11 H 14 ClN 3 O 4 S 3 2 acarbose C 25 H 43 NO 18 3 amiloride C 6 H 8 ClN 7 O 4 diazepam C 16 H 13 ClN 2 O 5 amfepramone C 13 H 19 NO 6 amphetamine C 9 H 13 N 7 bupropion C 13 H 18 ClNO 8 triamterene C 12 H 11 N 7 9 orlistat C 29 H 53 NO 5 10 oxethazaine C 28 H 41 N 3 O 3 11 bambuterol C 18 H 29 N 3 O 5 12 phenobarbital C 12 H 12 N 2 O 3 13 phenylalanine (DL), (L) C 9 H 11 NO 2 14 phenylpropanolamine C 9 H 13 NO 15 phentermine C 10 H 15 N 16 benfluorex C 19 H 20 F 3 NO 2 17 phenmetrazine C 11 H 15 NO 18 phendimetrazine C 12 H 17 NO 19 phenytoin C 15 H 12 N 2 O 2 20 isoxsuprine C 18 H 23 NO 3 21 phenformin C 10 H 15 N 5 22 ethyl 4-aminobenzoate C 9 H 11 NO 2 23 bisacodyl C 22 H 19 NO 4 24 benzfetamine C 17 H 21 N 25 bendroflumethiazide C 15 H 14 F 3 N 3 O 4 S 2 26 benzthiazide C 15 H 14 ClN 3 O 4 S 3 27 probenecid C 13 H 19 NO 4 S 28 bumetanide C 17 H 20 N 2 O 5 S 29 theophylline C 7 H 8 N 4 O 2 30 acetazolamide C 4 H 6 N 4 O 3 S 2 31 emodin C 15 H 10 O 5 32 usnic acid C 18 H 16 O 7 33 dobutramine C 12 H 20 O 34 metformin C 4 H 11 N 5 35 A sennoside A C 42 H 38 O B sennoside B C 42 H 38 O C sennoside C C 42 H 40 O D sennoside D C 42 H 40 O A sennidin A C 30 H 18 O B sennidin B C 30 H 18 O 10

4 续表 1 CAS 41 fenoterol C 17 H 21 NO 4 42 phenothiazine C 12 H 9 NS 43 phenolphthalein C 20 H 14 O 4 44 phentolamine C 17 H 19 N 3 O 45 furosemide C 12 H 11 ClN 2 O 5 S 46 fenfluramine C 12 H 16 F 3 N 47 fluoxetine C 17 H 18 F 3 NO 48 cyclothiazide C 14 H 16 ClN 3 O 4 S 2 49 gemfibrozil C 15 H 22 O 3 50 methyl amphetamine C 10 H 15 N 51 methylephedrine C 11 H 17 NO 52 thyroxine (D), (L) C 15 H 11 O 4 I 4 N 53 caffeine C 8 H 10 N 4 O 2 54 theobromine C 7 H 8 N 4 O 2 55 clenpenterol C 13 H 20 Cl 2 N 2 O 56 clenbuterol C 12 H 18 Cl 2 N 2 O 57 ractopamine C 18 H 23 NO 3 58 rimonabant C 22 H 21 Cl 3 N 4 O 59 sulbutiamine C 32 H 46 N 8 O 6 S 2 60 lorcaserin C 11 H 14 ClN 61 chlorphentermine C 10 H 14 ClN 62 clobenzorex C 16 H 18 ClN 63 clorprenaline C 11 H 16 ClNO 64 clopamide C 14 H 20 ClN 3 O 3 S 65 chlorothiazide C 7 H 6 ClN 3 O 4 S 2 66 chlorthalidone C 14 H 11 ClN 2 O 4 S 67 spironolactone C 24 H 32 O 4 S 68 ephedrine C 10 H 15 NO 69 mabuterol C 13 H 18 ClF 3 N 2 O 70 mapenterol C 14 H 20 ClF 3 N 2 O 71 mazindol C 16 H 13 ClN 2 O 72 metolazone C 16 H 16 ClN 3 O 3 S 73 modafinil C 15 H 15 NO 2 S 74 nefazodone C 25 H 32 ClN 5 O 2 75 paroxetine C 19 H 20 FNO 3 76 meperidine C 15 H 21 NO 2 77 penbutolol C 18 H 29 NO 2 78 propranolol C 16 H 21 NO 2 79 hydroflumethiazide C 8 H 8 F 3 N 3 O 4 S 2 80 hydrochlorothiazide C 7 H 8 ClN 3 O 4 S 2

5 5, : 1589 续表 1 CAS 81 cathine hydrochloride C 9 H 13 NO 82 salbutamol C 13 H 21 NO 3 83 sertraline C 32 H 38 N 4 O 12 S 3 84 strychnine C 21 H 22 N 2 O 2 85 salicin C 13 H 18 O 7 86 terbutaline C 12 H 19 NO 3 87 topiramate C 12 H 21 NO 8 S 88 torasemide C 16 H 20 N 4 O 3 S 89 tulobuterol C 12 H 18 ClNO 90 pseudoephedrine C 10 H 15 NO 91 penfluridol C 28 H 27 ClF 5 NO 92 sibutramine C 17 H 26 ClN 93 cimbuterol C 13 H 19 N 3 O 94 sildenafil C 22 H 30 N 6 O 4 S 95 cimaterol C 12 H 17 N 3 O 96 citalopram C 20 H 21 FN 2 O 97 synephrine C 9 H 13 NO 2 98 brombuterol C 12 H 18 Br 2 N 2 O 99 nicotinamide C 6 H 6 N 2 O 100 bergenin C 14 H 16 O ethacrynic acid C 13 H 12 Cl 2 O indapamide C 16 H 16 ClN 3 O 3 S 103 yohimbine C 21 H 26 N 2 O L-carnitine C 7 H 15 NO zonisamide C 8 H 8 N 2 O 3 S 106 2,4-2,4-dinitrophenol C 6 H 4 N 2 O ,3,5-3,3,5 -triiodo-l-thyronine C 15 H 12 I 3 NO ,3,5-3,3,5-triiodo-l-thyronine C 15 H 12 I 3 NO ,5-3,5-diiodo-l-thyronine C 15 H 13 I 2 NO N- n-di-desmethyl sibutramine C 15 H 22 ClN 111 N- n-mono-desmethyl sibutramine C 17 H 26 CIN 3.1 样品前处理, ( )3,,,,,,,, 固 - 液萃取 - 2 :

6 ,,,,, -,,,,,, (3600 g, 5 min) (16000 g, 3 min)2, (liquid chromatography-mass spectrometry, LC-MS) [10], HPLC [2], 30 min, r/min 5 min, , 0.22 μm [60] 液 - 液萃取 - ( ),, : (9:1, V:V) (3600 g, 5 min),,, (16000 g, 3 min), LC-MS [10] -, 解吸附电晕束电离 (atmosphere pressure chemical ionization, APCI),,,,,,, (DCBI-MS), [59] QuEChERS, QuEChERS, (solid phase extraction, SPE),,, β-, 6 (cleanert alumina-n cleanert C18 florisil cleanert pestic carb cleanert NH 2 cleanert PSA), cleanert pestic carb, [61] 其他前处理,,,, [12], 0.45 μm, HPLC [2], T4,, T4, [62],, T4 ELISA, T4,,, LC-MS 3.2 分离和检测方法,,,,, LC-MS NMR 11-desisobutyl-11-benzylsibutramine [18] 薄层色谱法, ; [4,40,54,63], 3, ; 30 min 60 min [4], 225 nm - - (10:1:0.1, V:V:V), ( 60 F254), 250~2000 ng [8] - - (9:1:0.3, V:V:V),,, 1~6 mg, 190 ng 634 ng [63] [40],, (254 nm), (2 μg),, (0.4 μg) [25], 254 nm 20 cm 10 cm HPTLC, 60F254, - - (10:1:0.1, V:V:V ) 3 250~2000 ng [8] 液相色谱法,

7 5, : 1591 HPLC, [4,13,20,30,31,42,50,64] [8] MS [2,4,24,27,29,30,35,36,40,41,43,44,49,51,52-55,64,65],,,,, 200~500 nm, nm nm nm ; 200 nm, 222 nm [42], HPLC-DAD,, Alltina C 18 : Ⅰ mol/l ( 0.1% )(12:88, V:V), Ⅱ mol/l ( 0.1% ) (60:40, V:V) 215 nm, 550 nm, 190~600 nm [50] Agilent Zorbax SB C 18 (200 mm 4.6 mm, 5 μm), 0.02 mol/l ( 0.1% )- (20:80, V:V),, 225 nm, [25] UHPLC-DAD ph 5.0, Vision HT C 18 -B(2 mm 100 mm, 1.5 μm) [13],, 225 nm [50], 275 nm [31],,,, [30] 毛细管电泳, [12,55] Cianchino [12] 4, 4,,, 2%,,,,,, [56] 离子淌度光谱法, [14,16], [14], (limit of detection, LOD) 2 ng IMS,,, 气相色谱法,, Parr - (gas chromatography-mass spectrometer, GC-MS) [3] 30 μg, (, 30 μg 3 ) (20 μg) X 射线衍射 X, (coulometric electrode array, CEAD) (time-of-flight mass spectrometry, TOF-MS), X (X-ray powder diffraction, XRPD) [58] X [64] 酶联免疫法 (ELISA) ELISA,, ELISA,, [62] 核磁共振,, diffusion ordered spectroscopy (DOSY) 1 H-nuclear magnetic resonance (NMR) DOSY-COSY

8 H-NMR, 20, 14,, 8, 5, 1 [22] 其他 (flow inject, FI),, (flow inject tandem mass spectrometry, FI-MS/MS) N- N- [60],, LC-MS/MS, 11-desisobutyl-11- benzylsibutramine [18] LC-DAD-MS n acomplia,, NIR, 2, X (X-ray diffraction, XRD), N- N- [64] 4 发展趋势,, (direct analysis in real time, DART) /,, ( ),,,,,, -,, -, mg/g,,,,,, 5 总结,,,,, -,, 参考文献 [1] [DB/OL] ( ). [2] Huang ZQ, Xiao S, Huang DL, et al. Simultaneous determination of sibutramine and N-di-desmethylsibutramine in dietary supplements for weight control by HPLC-ESI-MS [J]. J Chromatogr Sci, 2008, 46(8): [3] Parr MK, Koehler K, Geyer H, et al. Clenbuterol marketed as dietary supplement [J]. Bio Med Chromatogr, 2008, 22(3): [4],. [J]., 2013, (21): Liu RB, Liu CH. The rapid determination of illegal adulterants of sibutramine hydrochloride in weight reducing dietary supplement [J]. Guide Chin Med, 2013, (21): [5],,,. LC-MS/MS 11 [J]., 2009, 23(4): Li D, Wen HM, Cui FC, et al. Screening for 11 slim chemical compositions in health food by LC-MS/MS [J]. Chin Pharm Aff, 2009, 23(4): [6],,, [J]., 2010, (5): Sun XG, Zhao R, Zhang Z, et al. Survey on illegal addition drugs in weight-loss foods in [J]. Chin J Food Hyg, 2010, (5): [7],,, [J]., 2008, 28(8): Wang K, Hu Q, Cui YL, et al. Detection of 28 chemical drugs added illegally into slimming traditional Chinese medicines and health food by liquid chromatography-ion trap mass spectrometry method [J]. Chin J Pharm Anal, 2008, 28(8): [8] Ariburnu E, Uludag MF, Yalcinkaya H, et al. Comparative determination of sibutramine as an adulterant in natural slimming products by HPLC and

9 5, : 1593 HPTLC densitometry [J]. J Pharm Biomed Anal, 2012, 64 65(4): [9] Armenta S, Garrigues S, De IGM, et al. Analysis of ecstasy in oral fluid by ion mobility spectrometry and infrared spectroscopy after liquid-liquid extraction [J]. J Chromatogr A, 2015, 1384: 1 8. [10] Bogusz MJ, Hassan H, Al-Enazi E, et al. Application of LC-ESI-MS-MS for detection of synthetic adulterants in herbal remedies [J]. J Pharm Biomed Anal, 2006, 41(2): [11] Champagne AB, Emmel KV. Rapid screening test for adulteration in raw materials of dietary supplements [J]. Vib Spectr, 2011, 55(2): [12] Cianchino V, Acosta G, Ortega C, et al. Analysis of potential adulteration in herbal medicines and dietary supplements for the weight control by capillary electrophoresis [J]. Food Chem, 2008, 108(3): [13] Deconinck E, Verlinde K, Courselle P, et al. A validated ultra high pressure liquid chromatographic method for the characterisation of confiscated illegal slimming products containing anorexics [J]. J Pharm Biomed Anal, 2011, 59(1): [14] Dunn JD, Gryniewicz-Ruzicka CM, Kauffman JF, et al. Using a portable ion mobility spectrometer to screen dietary supplements for sibutramine [J]. J Pharm Biomed Anal, 2011, 54(3): [15] Greenway F, De JL, Martin C, et al. Dietary herbal supplements with phenylephrine for weight loss [J]. J Med Food, 2006, 9(4): [16] Dunn JD, Gryniewicz-Ruzicka CM, Mans DJ, et al. Qualitative screening for adulterants in weight-loss supplements by ion mobility spectrometry [J]. J Pharm Biomed Anal, 2012, 71(6): [17] Major GC, Doucet E, Jacqmain M, et al. Multivitamin and dietary supplements, body weight and appetite: results from a cross-sectional and a randomised double-blind placebo-controlled study [J]. Brit J Nutr, 2008, 99(05): [18] Mans DJ, Gucinski AC, Dunn JD, et al. Rapid screening and structural elucidation of a novel sibutramine analogue in a weight loss supplement: 11-Desisobutyl-11-benzylsibutramine [J]. J Pharm Biomed Anal, 2013, 83(1): [19] Ponnuru VS, Challa BR, Nadendla RR. Quantification of sibutramine and its two metabolites in human plasma by LC-ESI-MS/MS and its application in a bioequivalence study [J]. J Pharm Anal, 2012, 2(4): [20] Rebiere H, Guinot P, Civade C, et al. Detection of hazardous weight-loss substances in adulterated slimming formulations using ultra-high-pressure liquid chromatography with diode-array detection [J]. Food Addit Contam A, 2012, 29(2): [21] Reyes NR, Oliver TL, Klotz AA, et al. Similarities and differences between weight loss maintainers and regainers: aqualitative analysis [J]. J Acad Nutr Diet, 2012, 112(4): [22],,,. [J]., 2010, 22(5): Sun XG, Zhao R, Zhang Z, et al. Survey on the illegal drugs added in health food with losing weight, relieving physical fatigue and assist-reducing glycemia functions [J]. Chin J Food Hyg, 2010, 22(5): [23] Vaysse J, Balayssac S, Gilard V, et al. Analysis of adulterated herbal medicines and dietary supplements marketed for weight loss by DOSY 1H-NMR [J]. Food Addit Contam A, 2010, 27(7): [24] Wang J, Chen B, Yao S. Analysis of six synthetic adulterants in herbal weight-reducing dietary supplements by LC electrospray ionization-ms [J]. Food Addit Contam A, 2008, 25(7): [25],,. [J].,2008, 29(2): Cao L, Zhang YL, Wang BZ. Identification and determination of illegal adding of sibutramine hydrochloridein diet pills of traditional Chinese medicine for health care [J]. Food Chem, 2008, 29(2): [26], 喆,,. [J].,2009, 29(4): Che BQ, Zhang Z, Huang XJ, et al. HPLC-MS/MS identification of antiobesities in traditional Chinese medicine and health foods [J]. Chin J Pharm Anal, 2009, 29(4): [27],. HPLC/ESI-MS [J]., 2010, 22(1): Chen Z, Wu DD. Determination of N-di-Desmethylsibutramine with HPLC/ESI-MS in slimming health food products [J]. Chin J Food Hyg, 2010, 22(1): [28],. / [J]., 2010, 21(2): Chen Z, Wu DD. Determination of sibutramine hydrochloride in weight-loss healthy food by HPLC/electrospray ionization-ms [J]. Chem Res, 2010, 21(2): [29], 甦,,. LC-MS [J]., 2011, 21(8): Hu Q, Zhang S, Jian HL, et al. Identification of sibutramine and its derivatives added illegally into functional food by LC-MS n trap [J]. Chin J Health Lab Technol, 2011, 21(8): [30],,. [J]., (2): Huang NJ, Yang WH, Huang YB. Study on quick screening test for chemicals such as phenolphthalein and sibutramine hydrochloride illegally mixed into anti-obesity Chinese patent medicine, healthcare food and food stuff [J]. Food Drug, 2011, 13(2): [31],,. HPLC [J]., 2011, 30(1): Huang YB, Huang NJ, Yang WH. Study on determination of illegally added phenolphthalein in slimming health food by HPLC [J]. Qilu Pharm Aff, 2011, 30(1): [32],,,. - [J]., 2010, (2): Ma W, Chen DD, Wang HB, et al. Determination of phenolphthalein added in the weight-loss functional foods by ultrasonication-high performance liquid chromatography tandem mass spectrometry [J]. Food Ind, 2010, (2): [33],,,. - [J]., 2011, 32(2): Ma W, Dai HH, Zhang YC, et al. Determination of illegal drug benzocaine added in weight-loss functional foods by HPLC-MS/MS [J]. Sci Technol Food Ind, 2011, 32(2): [34],,,. -

10 [J]., 2010, 28(1): Ma W, Ma Q, Fu L, et al. Simultaneous determination of rimonabant and orlistat illegally added in the weight-loss functional foods by high performance liquid chromatography tandem mass spectrometry [J]. Chin J Chromatogr, 2010, 28(1): [35],,, [J]., 2009, 37(11): Ma W, Peng T, Zhu MD, et al. Simultaneous determination of 11 appetite suppressants in weight-loss functional foods by accelerated solvent extraction-high performance liquid chromatography tandem mass spectrometry [J]. Chin J Anal Chem, 2009, 37(11): [36],,. UPLC-MS/MS 36 [J]. 2013, 33(12): Ou BL, Zhang HW, Xu HX. Determination of 36 chemicals added into traditional Chinese medicines and health care products UPLC-MS/MS [J]. Chin J Pharm Anal, 2013, 33(12): [37],,,. HPLC-UV-ESI-MS [J]., 2006, 35(3): Xiao S, Zhu XL, Chen B, et al. Determination of orlistat in health food for controlling body weight by high performance liquid chromatography electrospray spectrometry [J]. J Hyg Res, 2006, 35(3): [38],,,. [J]., 2013, 27(12): Wan LC, Wang D, Ding YP, et al. Study on the rapid identification of adulterants in health food with weight reducing function [J]. Chin Pharm Aff, 2013, 27(12): [39],,, 25 [J]., 2014, 32(2): Wang JW, Huang XL, Cao J, et al. Simultaneous determination of 25 illegally added drugs in diet health foods by ultra-high performance liquid chromatography [J]. Chin J Chromatogr, 2014, 32(2): [40],,. [J]., 2011, 14(4): Wu ZJ, Liu SP, Guo SM. Exploratory detection of chemical drugs phenolphthalein and sibutramine hydrochloride added illegally into slimming food and health food [J]. China Pharm, 2011, 14(4): [41],,. [J]., 2011, 20(14): Xue LB, Ou BL, Shen CY, et al. Determination of sibutramine hydrochloride and phenolphthalein illegally added in slimming health foods by UPLC-MS/MS [J]. China Pharm, 2011, 20(14): [42],,,. HPLC [J]., 2012, (1): Yan B, Liu TH, Hu HS, et al. Simultaneous determination of four species of contraband medicine components in health food for controlling body weight by HPLC [J]. Mod Sci Instrum, 2012, (1): [43],,. HPLC-MS 4 [J]., 2006, 16(5): Yan H, Li XY, Peng FQ. Simultaneous determination of 4 kinds of chemical drug in slimming foods by HPLC-mass spectrometry [J]. J Mod Food Pharm, 2006, 16(5): [44],,,. [J]., 2010, 31(14): Yang CH, Wang W, Li G, et al. Determination of total amount of sibutramine and its active metabolites in weight-reducing food [J]. Food Sci, 2010, 31(14): [45],,. [J]., 2010, 08(34): Yang WH, Huang YB, Huang NJ. Test for sibutramine hydrochloride illegally mixed into anti-obesity Chinese patent medicine, health care food and food stuff [J]. Guide Chin Med, 2010, 08(34): [46],,. [J]., 2012, 30(6): Yao L, Chen JG, Chen D. Quick screening test for chemicals illegally mixed into anti-obesity healthcare food [J]. J Huaihai Med, 2012, 30(6): [47],. [J]., 2010, 33(3): Yu L, Chen H. Determination of illegal mixing of sibutramine hydrochloride in traditional Chinese medicine for health care [J]. Acta Acad Med Zunyi, 2010, 33(3): [48],,. HPLC-MS/MS 6 [J]., 2009, 44(17): Zeng XL, He SH, Huang XD, et al. Identification of six anti-obesity chemical drugs added into traditional Chinese medicines and health foods by liquid chromatography-ion trap mass spectrometry method [J]. Chin Pharm J, 2009, 44(17): [49]. LC-MS/MS [J]., 2011, 1(18): Zhang T. Analysis of phenolphthalein illegally added into functional food by LC-MS/MS [J]. China Med Pharm, 2011, 1(18): [50],,,. HPLC-DAD 10 [J]., 2012, 21(2): Zhang XD, Fu XY, Chen J, et al. A HPLC-DAD spectrum library for rapidly detecting 10 anti-obesity chemicals illegally adulterated intraditional Chinese medicines and healthy foods [J]. Chin J New Drugs, 2012, 21(2): [51],, [J]., 2009, 19(11): Zhu B, Yang Z, Wang ZW. Detection of 10 slimming drugs added illegally into functional foods by high performance liquid chromatography ion trap mass spectrometry [J]. Chin J Health Lab Technol, 2009, 19(11): [52]. UPLC/S/MS [J]., 2011, 11(9): Pan ZF. Determination of caffeine, phenolphthalein and sibutramine illegally added to weight loss functional food by UPLC/MS/MS [J]. China Trop Med, 2011, 11(9): [53],,. UPLC-MS/MS [J]., 2011, 46(20): Shen GF, Zhu J, Qiu YJ. Determination of sibutramine and its desmethyl derivatives added in slimming foods by UPLC-MS /MS [J]. Chin Pharm J,

11 5, : , 46(20): [54]. [J]., 2009, 11(9): Shi BL. Quick identification test for sibutramine mixed into anti-obesity health care food [J]. Med Pharm World, 2009, 11(9): [55],. [J]., 2010, 19(18): Wu WT, Li L. Determination of illegally added sibutramine hydrochloride in health food [J]. China Pharm, 2010, 19(18): [56],,,. 7 [J]., 2011, 39(11): Li Y, Xue F, Wang Y, et al. Simultaneous determination of seven adulterants in slimming functional foods by high performance capillary electrophoresis [J]. Chin J Anal Chem, 2011, 39(11): [57] Deconinck E, Cauwenbergh T, J Bothy L, et al. Detection of sibutramine in adulterated dietary supplements using attenuated total reflectance-infrared spectroscopy [J]. J Pharm Biomed Anal, 2014, 100(9): [58] Stypułkowska K, Błażewicz A, Maurin J, et al. X-ray powder diffractometry and liquid chromatography studies of sibutramine and its analogues content in herbal dietary supplements [J]. J Pharm Biomed Anal, 2011, 56(5): [59],,,. [J]., 24(4): Zhao Y, Wang H, Zhu HG, et al. Detection of illegal synthetic drugs in weight reducing dietarysupplements by hybrid of DCBI-MS and HPLC-UV [J]. Chin J Food Hyg, 24(4): [60] Song F, Monroe D, El-Demerdash A, et al. Screening for multiple weight loss and related drugs in dietary supplement materials by flow injection tandem mass spectrometry and their confirmation by liquid chromatography tandem mass spectrometry [J]. J Pharm Biomed Anal, 2014, 88(25): [61] Li JH, Zhang ZH, Liu X, et al. Analysis of fourteen β-agonists in weight-reducing dietary supplements using QuEChERS-based extraction followed by high resolution UHPLC-MS [J]. Food Anal Method, 2014, (7): [62] Mikami E, Ohno T, Matsumoto H, et al. Detection of thyroxine in dietary supplements using an enzyme-linked immunosorbent assay [J]. J Health Sci, 2003, 49(6): [63] Phattanawasin P, Sotanaphun U, Sukwattanasinit T, et al. Quantitative determination of sibutramine in adulterated herbal slimming formulations by TLC-image analysis method [J]. Forensic Sci Int, 2012, 219(1 3): [64] Venhuis BJ, Vredenbregt MV, Kaun N, et al. The identification of rimonabant polymorphs, sibutramine and analogues of both in counterfeit acomplia bought on the internet [J]. J Pharm Biomed Anal, 2011, 54(1): 作者简介 ( 责任编辑 : 杨翠娜 ) 李建辉, 硕士, 工程师, 主要研究方向为食品检测 [email protected] 张朝晖, 博士, 高级工程师, 主要研究方向为食品检测 [email protected]