Bìa tạp chí



Simultaneous determination of sibutramine and its derivatives in weight loss dietary supplements by LC-MS/MS

Duong Thi Mai Hoa Pham Thi Ngoc Mai Cao Cong Khanh Nguyen Thi Hong Ngoc Mac Thi Thanh Hoa Tran Hung Son Nguyen Thi Van Anh Le Thi Hong Hao
Published 06/19/2020

Article Details

How to Cite
Duong Thi Mai Hoa, Pham Thi Ngoc Mai, Cao Cong Khanh, Nguyen Thi Hong Ngoc, Mac Thi Thanh Hoa, Tran Hung Son, Nguyen Thi Van Anh, Le Thi Hong Hao. "Simultaneous determination of sibutramine and its derivatives in weight loss dietary supplements by LC-MS/MS". Vietnam Journal of Food Control. vol. 3, no. 2 (en), pp. 104-114, 2020

Main Article Content


The liquid chromatography tandem mass spectrometry method (LC-MS/MS) was used to determine the content of sibutramine (SB), N-desmethyl sibutramine (DSB) and N-didesmethyl sibutramine (DDSB) illegaly mixed in weight loss dietary supplements. Sibutramine and its derivatives were extracted by methanol; impurities in the extract were removed by graphitized carbon black (GCB) adsorbent. The chromatographic separation of analytes took place on C18 column (100 mm x 2.1 mm, 3.5 µm) with a gradient mobile phase of acetonitrile and 2 mM ammonium acetate in 0.1% formic acid solution. Multiple reaction monitoring (MRM) in the positive mode was used to detect and quantify SB, DSB and DDSB at m/z 279.9/124.8; 266.0/124.8 and 252.1/125.0, respectively. The method was validated following the AOAC requirements for specificity, repeatability and recovery. Calibration curves lineared from 0.002 to 0.1 µg/mL for SB, DSB and DDSB. The method was successfully applied to determine the content of SB, DSB and DDSB in weight loss dietary supplements that were randomly collected from phamacies in Hanoi of three formulations of hard capsule, soft capsule and teabag. The results shown that six samples had SB and DSB with the content in the range of 0.817 - 31.7 mg/g.


sibutramine, N-desmethyl sibutramine, N-didesmethyl sibutramine, weight lossdietary supplement, LC-MS/MS


[1] A. Krivohlavek, I. Žuntar, M. Ivešić, I. M. Andačić, S. Šikić, and M. Vrebčević, “Sibutramine in slimming food supplements on the Croatian market determined by validated high­pressure liquid chromatographyelectrospray tandem mass spectrometry method”, Journal of Food and Nutrition Research, vol. 55, pp. 222­228, 2016.
[2] E. P. Gueorguieva, K. Ivanov, S. Gueorguiev, A. Mihaylova, V. Madzharov and S. Ivanova, “Detection of sibutramine in herbal food supplements by UHPLC/HRMS and UHPLC/MS­MS”,Biomedical Research, vol. 29, no.14, pp. 3006­3009, 2018
[3] H. M. Yano, F. F. Farias, M. B. D. Bianco and L. M. Trujllo, “Determination of the Sibutramine Content of Dietary Supplements Using LC­ESI­MS/MS”, Journal of Pharmaceutical Analysis. 32 (8): 1164­1169, 2013.
[4] V. S. Ponnuru, B.R. Challa and R. Nadendla, “Quantification of sibutramine and its two metabolites in human plasma by LC­ESI ­ MS/MS and its application in a bioequivalence study”, Journal of Pharmaceutical Analysis, vol. 2, no. 4, pp. 249­257, 2012.
[5] P. Zou, S. S­Y. Oh, K.­H. Kiang, M­Y. Low and B.C. Bloodworth, “Detection of sibutramine, its two metabolites and one analogue in a herbal product for weight loss by liquid chromatography triple quadrupole mass spectrometry and time­of­flight mass spectrometry”, Rapid Communications in Mass Spectrometry, vol. 21, no. 4, pp. 614­618, 2007.
[6] J. Wang, B. Chen and S. Yao, “Analysis of six synthetic adulterants in herbal weight­reducing dietary supplements by LC electrospray ionization­MS”, Food Additives & Contaminants: Part A, vol. 25, no. 7, pp. 822­830, 2008.
[7] J. Chen, W. Lu, Q. Zhang and X. Jiang, “Determination of the active metabolite of sibutramine by liquid chromatography­electrospray ionization tandem mass spectrometry”, Journal of Chromatography B, vol. 785, pp. 197­203, 2003.
[8] S. H. Roh, Y.P. Kang, S. Park, Y. Huh, J. Lee, J.H. Park, D. Kim and S.W. Kwon, “Determination of tadalafil and N­desmethylsibutramine in health and dietary supplements using ultraperformance liquid chromatography (UPLC) coupled with quadrupole­time­of­flight mass spectrometry (QTOF MS)”, Food Additives and Contaminants, vol. 28, no. 11, pp. 1475­1482, 2011.
[9] E. Ariburnu, M. F. Uludag, H. Yalcinkaya and E. Yesilada, “Comparative determination of sibutramine as an adulterant in natural slimming product by HPLC and HPTLC densitometry”, Journal of Pharmaceutical and Biomedical Analysis, vol. 64­65, pp. 77­81, 2012.
[10] Z. Huang, S. Xiao, D. Luo, Bo Chen and S. Yao, “Simultaneous Determination of Sibutramine and N­Di­desmethylsibutramine in Dietary Supplements for Weight Control by HPLC­ESI­MS”, Journal of Chromatographic Science, vol. 46, no. 8, pp. 707­711, 2008.
[11] M. Chorilli, R. Bonfilio, R. S. Chicarelli and H. R. N. Salgado, “Development and validation of an analytical method by PR­HPLC for quantification of sibutramine in pharmaceutical capsule”, Analytical Methods, vol. 3, pp. 985­990, 2011.
[12] Y. Chena, L. Zhaob, F. Lua, Y. Yuc, Y. Chaia and Y. Wua, “Determination of synthetic drugs used to adulterate botanical dietary supplements using QTRAP LC­MS/MS”, Food Additives and Contaminants, vol. 26, no. 5, pp. 595­603, 2009.
[13] F. V. Sardela, M. T. R. Motta, M. C. Padilha, H. M. G. Pereira and F. R. Aquino Neto, “Analysis of sibutramine metabolites as Ntrifluoroacetamide and O­trimethylsilyl derivatives by gas chromatography­mass spectrometry in urine”, Journal of Chromatogr B, vol. 877, no. 27, pp. 3003­3011, 2009.
[14] S. Strano­Rossi, C. Colamonici and F. Botre, “Detection of sibutramine administration: a gas chromatography/mass spectrometry study of the main urinary metabolites”, Rapid Communication in Mass Spectrometrometry, vol. 21, no. 2, pp. 79­88, 2007.
[15] P. Zou, S. S­Y. Oh, K­H. Kiang, M­Y. Low and B. C. Bloodword, “Detection of sibutramine,its two metabolites and one analogue in a herbal product for weight loss by liquid chromatography triple quadrupole mass spectrometry and time­of­flight mass spectrometry”, Rapid Communication in Mass Spectrometrometry, vol. 21, pp. 614­618, 2007.
[16] N. T. Luyện, “Xác định chất cấm Sibutramine trong thực phẩm chức năng giảm béo bằng phương pháp HPLC”, Luận văn Thạc sỹ, Đại học Quốc gia Hà Nội, Việt Nam, 2014.
[17] T. Kamadi, I. Fidrianny, Amirmusadad, “Development of analytical method for identification of sibutramine in traditional medicine using solid phase extraction: high performance liquid chromatography”, Asian Journal of Pharmaceutical and Clinical Research, vol 9, no. 6, pp. 201­209, 2016.