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Current Analytical Chemistry

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ISSN (Print): 1573-4110
ISSN (Online): 1875-6727

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Research Article

Use of Fe3O4@MPTMS-Dithizone Magnetic Nanoparticles as Solid Phase Sorbent for Sensitive Analysis of Sibutramine Molecules in Herbal Slimming Products

Author(s): Özge Demir, Halil İbrahim Ulusoy*, Ümmügülsüm Polat and Songül Ulusoy

Volume 19, Issue 6, 2023

Published on: 19 July, 2023

Page: [472 - 481] Pages: 10

DOI: 10.2174/1573411019666230703141135

Price: $65

Abstract

Background: A new enrichment and sensitive determination method, which includes HPLCDAD analysis after Magnetic Solid Phase Extraction (MSPE), has been developed for trace analysis of Sibutramine molecules in herbal slimming products. Sibutramine is one of the most adulterated drug molecules in herbal products.

Method: In the proposed method, Sibutramine molecules were pre-concentrated by using Fe3O4@MPTMS-Dithizone magnetic sorbent synthesized in our laboratory. Desorption of Sibutramine molecules from the sorbent phase was carried out by using acetonitrile: methanol (1:1) solvent in the presence of pH 8.0 buffer before chromatographic determinations.

Results: Analytical parameters of the method, such as linear range, enrichment factor, and determination limit, were determined after optimizing experimental variables such as interaction time, desorption solvent, pH, etc. The sibutramine molecule was analyzed by isocratic elution of acetonitrile and KH2PO4 (pH 3.0, 0.05 M) (40:60) with a DAD detector at 223 nm wavelength. Limit of detection (LOD) value was calculated as 1.43 ng mL-1.

Conclusion: Relative standard deviations (RSD) were below 3.20% for determinations of model solutions, including 100 ng mL-1 of Sibutramine. Finally, the developed method has been applied to herbal slimming tea samples with quantitative recovery experiments.

Keywords: Sibutramine, magnetic solid phase extraction, HPLC, herbal slimming products, drug analysis, sibutramine molecule.

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[1]
An, H.; Sohn, H.; Chung, S. Phentermine, sibutramine and affective disorders. Clin. Psychopharmacol. Neurosci., 2013, 11(1), 7-12.
[http://dx.doi.org/10.9758/cpn.2013.11.1.7] [PMID: 23678348]
[2]
LeMURA, L.M.; Maziekas, M.T. Factors that alter body fat, body mass, and fat-free mass in pediatric obesity. Med. Sci. Sports Exerc., 2002, 34(3), 487-496.
[http://dx.doi.org/10.1097/00005768-200203000-00016] [PMID: 11880814]
[3]
Vega, G.L. Obesity, the metabolic syndrome, and cardiovascular disease. Am. Heart J., 2001, 142(6), 1108-1116.
[http://dx.doi.org/10.1067/mhj.2001.119790] [PMID: 11717620]
[4]
Romanucci, V.; Porcaro, P.; Di Marino, C.; De Marco, A. Scavenging effect of various extracts of the Gymnema sylvestre R. Br. and antioxidant activity of the isolated triterpenes. Rec. Nat. Prod., 2017, 12(1), 53-63.
[http://dx.doi.org/10.25135/rnp.01.17.05.098]
[5]
Seravalle, G.; Grassi, G. Obesity and hypertension. Pharmacol. Res., 2017, 122, 1-7.
[http://dx.doi.org/10.1016/j.phrs.2017.05.013] [PMID: 28532816]
[6]
Adan, R.; Vanderschuren, L.; Elafleur, S. Anti-obesity drugs and neural circuits of feeding. Trends Pharmacol. Sci., 2008, 29(4), 208-217.
[http://dx.doi.org/10.1016/j.tips.2008.01.008] [PMID: 18353447]
[7]
LeBlanc, M.; Thibault, L. Effect of sibutramine on macronutrient selection in male and female rats. Physiol. Behav., 2003, 80(2-3), 243-252.
[http://dx.doi.org/10.1016/j.physbeh.2003.07.010] [PMID: 14637222]
[8]
Waszkiewicz, N. Zalewska-Szajda, B.; Szajda, S.D.; Simonienko, K.; Zalewska, A.; Szulc, A.; Ładny, J.R.; Zwierz, K. Sibutramine-induced mania as the first manifestation of bipolar disorder. BMC Psychiatry, 2012, 12(1), 43.
[http://dx.doi.org/10.1186/1471-244X-12-43] [PMID: 22607132]
[9]
Ariburnu, E.; Uludag, M.F.; Yalcinkaya, H.; Yesilada, E. Comparative determination of sibutramine as an adulterant in natural slimming products by HPLC and HPTLC densitometry. J. Pharm. Biomed. Anal., 2012, 64-65, 77-81.
[http://dx.doi.org/10.1016/j.jpba.2012.02.004] [PMID: 22410500]
[10]
Yilmaz, E. Ulusoy, H.İ.; Demir, Ö.; Soylak, M. A new magnetic nanodiamond/graphene oxide hybrid (Fe3O4@ND@GO) material for pre-concentration and sensitive determination of sildenafil in alleged herbal aphrodisiacs by HPLC-DAD system. J. Chromatogr. B Anal. Technol. Biomed. Life Sci, 2018, 1084, 113-121.
[http://dx.doi.org/10.1016/j.jchromb.2018.03.030] [PMID: 29597037]
[11]
Gratz, S.R.; Flurer, C.L.; Wolnik, K.A. Analysis of undeclared synthetic phosphodiesterase-5 inhibitors in dietary supplements and herbal matrices by LC–ESI–MS and LC–UV. J. Pharm. Biomed. Anal., 2004, 36(3), 525-533.
[http://dx.doi.org/10.1016/j.jpba.2004.07.004] [PMID: 15522526]
[12]
Kruger, C.L.; Mann, S.W. Safety evaluation of functional ingredients. Food Chem. Toxicol., 2003, 41(6), 793-805.
[http://dx.doi.org/10.1016/S0278-6915(03)00018-8] [PMID: 12738185]
[13]
Yang, H.; Wurita, A.; Liu, J.; Wang, Y.; Hasegawa, K. Quantitation of sibutramine in human hair using gas chromatography–isotope dilution tandem mass spectrometry. Forensic Toxicol., 2022, 40(2), 366-373.
[http://dx.doi.org/10.1007/s11419-021-00609-3] [PMID: 36454400]
[14]
Carvalho, J.M.; Silva, A.R.; Cunha, A.L.M.C.; Aucélio, R.Q.; Alberti, A.L.M.; Leandro, K.C. Voltammetric determination of sibutramine in beverages and in pharmaceutical formulations. Quim. Nova, 2012, 35(5), 988-992.
[http://dx.doi.org/10.1590/S0100-40422012000500023]
[15]
Lima, A.B.; dos Santos, W.T.P.; Compton, R.G. Simple and sensitive determination of sibutramine in slimming tea beverages using a carbon screen‐printed electrode with adsorptive stripping voltammetry. Electroanalysis, 2019, 31(5), 975-980.
[http://dx.doi.org/10.1002/elan.201800888]
[16]
Hieu, T.Q.; Vi, P.P.H.; Phuong, P.K.; Bien, L.T.K.; Tan, N.T. Validation of the method for determination of Phenolphthalein and Sibutramine in weight-loss functional foods from Viet Nam by UPLC-MS/MS. Vietnam J. Chem., 2021, 59, 467-474.
[17]
Liu, Z.; Gao, Y.; Jin, L.; Jin, H.; Xu, N.; Yu, X.; Yu, S. Core–shell regeneration magnetic molecularly imprinted polymers-based sers for sibutramine rapid detection. ACS Sustain. Chem.& Eng., 2019, 7(9), 8168-8175.
[http://dx.doi.org/10.1021/acssuschemeng.8b06120]
[18]
Chaisiwamongkhol, K.; Labaidae, S.; Pon-in, S.; Pinsrithong, S.; Bunchuay, T.; Phonchai, A. Smartphone-based colorimetric detection using gold nanoparticles of sibutramine in suspected food supplement products. Microchem. J., 2020, 158, 105273.
[http://dx.doi.org/10.1016/j.microc.2020.105273]
[19]
Popescu, A.M.; Radu, G.L. Detection of adulterants by FTIR and GC-MS in herbal slimming food supplements. UPB Sci. Bull. Ser. B Chem. Mater. Sci., 2015, 77, 221-230.
[20]
Buchberger, W.W. Novel analytical procedures for screening of drug residues in water, waste water, sediment and sludge. Anal. Chim. Acta, 2007, 593(2), 129-139.
[http://dx.doi.org/10.1016/j.aca.2007.05.006] [PMID: 17543599]
[21]
Campone, L.; Piccinelli, A.L.; Celano, R.; Pagano, I.; Russo, M.; Rastrelli, L. Rapid and automated on-line solid phase extraction HPLC–MS/MS with peak focusing for the determination of ochratoxin A in wine samples. Food Chem., 2018, 244, 128-135.
[http://dx.doi.org/10.1016/j.foodchem.2017.10.023] [PMID: 29120760]
[22]
Giakisikli, G.; Anthemidis, A.N. Magnetic materials as sorbents for metal/metalloid preconcentration and/or separation. A review. Anal. Chim. Acta, 2013, 789, 1-16.
[http://dx.doi.org/10.1016/j.aca.2013.04.021] [PMID: 23856225]
[23]
Kabir, A.; Locatelli, M.; Ulusoy, H. Recent trends in microextraction techniques employed in analytical and bioanalytical sample preparation. Separations, 2017, 4(4), 36.
[http://dx.doi.org/10.3390/separations4040036]
[24]
Sarıkaya, M.; Ulusoy, H.I.; Morgul, U.; Ulusoy, S.; Tartaglia, A.; Yılmaz, E.; Soylak, M.; Locatelli, M.; Kabir, A. Sensitive determination of Fluoxetine and Citalopram antidepressants in urine and wastewater samples by liquid chromatography coupled with photodiode array detector. J. Chromatogr. A, 2021, 1648, 462215.
[http://dx.doi.org/10.1016/j.chroma.2021.462215] [PMID: 34000593]
[25]
Vuran, B.; Ulusoy, H.I.; Sarp, G.; Yilmaz, E.; Morgül, U.; Kabir, A.; Tartaglia, A.; Locatelli, M.; Soylak, M. Determination of chloramphenicol and tetracycline residues in milk samples by means of nanofiber coated magnetic particles prior to high-performance liquid chromatography-diode array detection. Talanta, 2021, 230, 122307.
[http://dx.doi.org/10.1016/j.talanta.2021.122307] [PMID: 33934773]
[26]
Vasconcelos, I.; Fernandes, C. Magnetic solid phase extraction for determination of drugs in biological matrices. Trends Analyt. Chem., 2017, 89, 41-52.
[http://dx.doi.org/10.1016/j.trac.2016.11.011]
[27]
Ulusoy, H.I. Applications of magnetic nanoparticles for the selective extraction of trace species from a complex matrix, 1st ed; Nova Scientific Publishers: New York, 2017.
[28]
Sobiech, M. Giebułtowicz, J.; Luliński, P. Application of magnetic core–shell imprinted nanoconjugates for the analysis of hordenine in human plasma-preliminary data on pharmacokinetic study after oral administration. J. Agric. Food Chem., 2020, 68(49), 14502-14512.
[http://dx.doi.org/10.1021/acs.jafc.0c05985] [PMID: 33227193]
[29]
Cui, Y.; Ding, L.; Ding, J. Recent advances of magnetic molecularly imprinted materials: From materials design to complex sample pretreatment. Trends Analyt. Chem., 2022, 147, 116514.
[http://dx.doi.org/10.1016/j.trac.2021.116514]
[30]
Cheng, G.; He, M.; Peng, H.; Hu, B. Dithizone modified magnetic nanoparticles for fast and selective solid phase extraction of trace elements in environmental and biological samples prior to their determination by ICP-OES. Talanta, 2012, 88, 507-515.
[http://dx.doi.org/10.1016/j.talanta.2011.11.025] [PMID: 22265534]
[31]
Elwakeel, K.Z.; Hamza, M.F.; Guibal, E. Effect of agitation mode (mechanical, ultrasound and microwave) on uranium sorption using amine- and dithizone-functionalized magnetic chitosan hybrid materials. Chem. Eng. J., 2021, 411, 128553.
[http://dx.doi.org/10.1016/j.cej.2021.128553]
[32]
Ma, J.; Zeng, Y.; Sun, M.; Zhang, M.; Zheng, W.; Zhang, C.; Wang, Q.; Xiao, Y.; Zhang, S. A superparamagnetic ZnFe2O4@NH2-SiO2@PMDI@ dithizone microspheres as an effective selective adsorbent for Pb2+ from wastewater. J. Environ. Chem. Eng., 2019, 7(1), 102874.
[http://dx.doi.org/10.1016/j.jece.2018.102874]
[33]
Moinfar, S.; Khodayari, A.; Sohrabnezhad, S.; Aghaei, A.; Jamil, L.A. MIL-53(Al)/Fe2O3 nanocomposite for solid-phase microextraction of organophosphorus pesticides followed by GC-MS analysis. Mikrochim. Acta, 2020, 187(12), 647.
[http://dx.doi.org/10.1007/s00604-020-04621-z] [PMID: 33165626]
[34]
Zhang, L.; Xiong, Z.; Zhang, L.; Yu, B.; Zhang, W. Magnetic nanoparticles coated with dithizone-modified chitosan for use in solid-phase extraction of copper(II). Anal. Methods, 2015, 7(5), 2050-2054.
[http://dx.doi.org/10.1039/C4AY02596B]
[35]
Chaikhan, P.; Udnan, Y.; Ampiah-Bonney, R.J.; Chaiyasith, W.C. Magnetic dispersive solid phase extraction using recycled-graphite for GO-Fe3O4-dithizone composite combined with FAAS for determination of lead in environmental samples. Anal. Sci., 2021, 37(7), 1015-1021.
[http://dx.doi.org/10.2116/analsci.20P383] [PMID: 33455961]
[36]
Ma, J.; Cheng, G.; Basov, S.; Zhang, S.; Ji, T. Extraction of Pb2+ from dilute solution by paramagnetic Fe3O4@SiO2@Clprsilica@ dithizone solid-phase nanoextractant. Desalination Water Treat., 2014, 52(40-42), 7898-7905, 7898-7905.
[http://dx.doi.org/10.1080/19443994.2013.833878]
[37]
Wierucka, M.; Biziuk, M. Application of magnetic nanoparticles for magnetic solid-phase extraction in preparing biological, environmental and food samples. Trends Analyt. Chem., 2014, 59, 50-58.
[http://dx.doi.org/10.1016/j.trac.2014.04.007]
[38]
Ulusoy, H.İ.; Gülle, S.; Yilmaz, E.; Soylak, M. Trace determination of vitamin B12 in food samples by using Fe3O4 magnetic particles including multi-walled carbon nanotubes and nanodiamonds. Anal. Methods, 2019, 11(40), 5108-5117.
[http://dx.doi.org/10.1039/C9AY01504C]
[39]
Mathon, C.; Ankli, A.; Reich, E.; Bieri, S.; Christen, P. Screening and determination of sibutramine in adulterated herbal slimming supplements by HPTLC-UV densitometry. Food Addit. Contam. Part A Chem. Anal. Control Expo. Risk Assess., 2014, 31(1), 15-20.
[http://dx.doi.org/10.1080/19440049.2013.861934] [PMID: 24215519]
[40]
Dal Molin, T.R.; Silveira, G.D.; Leal, G.C.; Müller, L.S.; Muratt, D.T.; Carvalho, L.M.; Viana, C. A new approach to ion exchange chromatography with conductivity detection for adulterants investigation in dietary supplements. Biomed. Chromatogr., 2019, 33(11), e4669.
[http://dx.doi.org/10.1002/bmc.4669] [PMID: 31368119]
[41]
Chen, J.; Lu, W.; Zhang, Q.; Jiang, X. Determination of the active metabolite of sibutramine by liquid chromatography–electrospray ionization tandem mass spectrometry. J. Chromatogr. B Analyt. Technol. Biomed. Life Sci., 2003, 785(2), 197-203.
[http://dx.doi.org/10.1016/S1570-0232(02)00818-8] [PMID: 12554132]
[42]
Ponnuru, V.S.; Challa, B.R.; Nadendla, R. Quantification of sibutramine and its two metabolites in human plasma by LC–ESI-MS/MS and its application in a bioequivalence study. J. Pharm. Anal., 2012, 2(4), 249-257.
[http://dx.doi.org/10.1016/j.jpha.2012.02.010] [PMID: 29403750]
[43]
Bhatt, J.; Shah, B.; Kambli, S.; Subbaiah, G.; Singh, S.; Ameta, S. Rapid and sensitive method for the determination of sibutramine active metabolites in human plasma by reversed-phase liquid chromatography-tandem mass spectroscopy. J. Chromatogr. Sci., 2007, 45(2), 91-96.
[http://dx.doi.org/10.1093/chromsci/45.2.91] [PMID: 17425138]
[44]
Suthar, A.P.; Dubey, S.A.; Patel, S.R. A validated specific reverse phase liquid chromatographic method for the estimation of sibutramine hydrochloride monohydrate in bulk drug and capsule dosage forms. Int. J. Chemtech Res., 2009, 1, 793-801.
[45]
Lahane, S.B.; Deokate, U.A.; Nawale, R.B. A stability indicating HPLC method for the determination of amodiquine hydrochloride. Int. J. Pharm. Sci. Rev. Res., 2014, 2, 8196-8199.

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