Determination of higenamine in dietary supplements by UHPLC/MS/MS method
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2017
Authors
Stajić, Ana
Anđelković, Marija
Dikić, Nenad

Rasić, J.
Vukašinović-Vesić, Milica
Ivanović, D.
Jančić-Stojanović, Biljana

Article (Published version)

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From 1st January 2017 higenamine was added on the WADA (World Anti-doping Agency) Prohibited list under S3 group beta-2 agonists as at all times banned substance for the athletes. The main origine of higenamine (or norcoclaurine) are different plants including Nandina domestica, Aconitum carmichaelii, Asarum heterotropioides, Galium divaricatum, Annona squamosa, Nelumbo nucifera etc. Higenamine main use is related to weight loss and it could be found (un)labeled in different dietary supplements. The objective of this study was development of sensitive and reliable UHPLC/MS/MS method for determination of higenamine in various dietary supplement samples. In order to obtain high method sensitivity, hydrophilic interaction liquid chromatography (HILIC) mode was applied. Separation was carried out on UHPLC Acquity BEH HILIC analytical column (2.1 mm x 100 mm, 1.7 mu m particle size). Mobile phase consisted of 0.1% formic acid in water and acetonitrile, respectively, was mixed in ratio of 30...:70, v/v. Flow rate was set at 0.2 mL min(-1). Quercetin was used as an internal standard. ESI (+) source ionization mode using multi reaction monitoring (MRM) mode was utilized and three ion transitions of higenamine were followed 272.08 -> 107.01, 272.08 -> 161.07 and 272.08 -> 77.08. Developed method was fully validated and applied for identification and quantification of higenamine in different dietary supplements. According to the results, the most of investigated supplements were free of higenamine, and on the other hand, presence of higenamine was confirmed in some samples while it was not declared on the label.
Keywords:
Higenamine / Dietary supplements / HILIC / UHPLC/MS/MSSource:
Journal of Pharmaceutical and Biomedical Analysis, 2017, 146, 48-52Publisher:
- Elsevier Science BV, Amsterdam
Funding / projects:
- Modelling of different chromatographic systems with chemometrical approach in pharmaceutical analysis (RS-172052)
DOI: 10.1016/j.jpba.2017.08.017
ISSN: 0731-7085
PubMed: 28850863
WoS: 000413283400007
Scopus: 2-s2.0-85028325402
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Institution/Community
PharmacyTY - JOUR AU - Stajić, Ana AU - Anđelković, Marija AU - Dikić, Nenad AU - Rasić, J. AU - Vukašinović-Vesić, Milica AU - Ivanović, D. AU - Jančić-Stojanović, Biljana PY - 2017 UR - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2869 AB - From 1st January 2017 higenamine was added on the WADA (World Anti-doping Agency) Prohibited list under S3 group beta-2 agonists as at all times banned substance for the athletes. The main origine of higenamine (or norcoclaurine) are different plants including Nandina domestica, Aconitum carmichaelii, Asarum heterotropioides, Galium divaricatum, Annona squamosa, Nelumbo nucifera etc. Higenamine main use is related to weight loss and it could be found (un)labeled in different dietary supplements. The objective of this study was development of sensitive and reliable UHPLC/MS/MS method for determination of higenamine in various dietary supplement samples. In order to obtain high method sensitivity, hydrophilic interaction liquid chromatography (HILIC) mode was applied. Separation was carried out on UHPLC Acquity BEH HILIC analytical column (2.1 mm x 100 mm, 1.7 mu m particle size). Mobile phase consisted of 0.1% formic acid in water and acetonitrile, respectively, was mixed in ratio of 30:70, v/v. Flow rate was set at 0.2 mL min(-1). Quercetin was used as an internal standard. ESI (+) source ionization mode using multi reaction monitoring (MRM) mode was utilized and three ion transitions of higenamine were followed 272.08 -> 107.01, 272.08 -> 161.07 and 272.08 -> 77.08. Developed method was fully validated and applied for identification and quantification of higenamine in different dietary supplements. According to the results, the most of investigated supplements were free of higenamine, and on the other hand, presence of higenamine was confirmed in some samples while it was not declared on the label. PB - Elsevier Science BV, Amsterdam T2 - Journal of Pharmaceutical and Biomedical Analysis T1 - Determination of higenamine in dietary supplements by UHPLC/MS/MS method VL - 146 SP - 48 EP - 52 DO - 10.1016/j.jpba.2017.08.017 ER -
@article{ author = "Stajić, Ana and Anđelković, Marija and Dikić, Nenad and Rasić, J. and Vukašinović-Vesić, Milica and Ivanović, D. and Jančić-Stojanović, Biljana", year = "2017", abstract = "From 1st January 2017 higenamine was added on the WADA (World Anti-doping Agency) Prohibited list under S3 group beta-2 agonists as at all times banned substance for the athletes. The main origine of higenamine (or norcoclaurine) are different plants including Nandina domestica, Aconitum carmichaelii, Asarum heterotropioides, Galium divaricatum, Annona squamosa, Nelumbo nucifera etc. Higenamine main use is related to weight loss and it could be found (un)labeled in different dietary supplements. The objective of this study was development of sensitive and reliable UHPLC/MS/MS method for determination of higenamine in various dietary supplement samples. In order to obtain high method sensitivity, hydrophilic interaction liquid chromatography (HILIC) mode was applied. Separation was carried out on UHPLC Acquity BEH HILIC analytical column (2.1 mm x 100 mm, 1.7 mu m particle size). Mobile phase consisted of 0.1% formic acid in water and acetonitrile, respectively, was mixed in ratio of 30:70, v/v. Flow rate was set at 0.2 mL min(-1). Quercetin was used as an internal standard. ESI (+) source ionization mode using multi reaction monitoring (MRM) mode was utilized and three ion transitions of higenamine were followed 272.08 -> 107.01, 272.08 -> 161.07 and 272.08 -> 77.08. Developed method was fully validated and applied for identification and quantification of higenamine in different dietary supplements. According to the results, the most of investigated supplements were free of higenamine, and on the other hand, presence of higenamine was confirmed in some samples while it was not declared on the label.", publisher = "Elsevier Science BV, Amsterdam", journal = "Journal of Pharmaceutical and Biomedical Analysis", title = "Determination of higenamine in dietary supplements by UHPLC/MS/MS method", volume = "146", pages = "48-52", doi = "10.1016/j.jpba.2017.08.017" }
Stajić, A., Anđelković, M., Dikić, N., Rasić, J., Vukašinović-Vesić, M., Ivanović, D.,& Jančić-Stojanović, B.. (2017). Determination of higenamine in dietary supplements by UHPLC/MS/MS method. in Journal of Pharmaceutical and Biomedical Analysis Elsevier Science BV, Amsterdam., 146, 48-52. https://doi.org/10.1016/j.jpba.2017.08.017
Stajić A, Anđelković M, Dikić N, Rasić J, Vukašinović-Vesić M, Ivanović D, Jančić-Stojanović B. Determination of higenamine in dietary supplements by UHPLC/MS/MS method. in Journal of Pharmaceutical and Biomedical Analysis. 2017;146:48-52. doi:10.1016/j.jpba.2017.08.017 .
Stajić, Ana, Anđelković, Marija, Dikić, Nenad, Rasić, J., Vukašinović-Vesić, Milica, Ivanović, D., Jančić-Stojanović, Biljana, "Determination of higenamine in dietary supplements by UHPLC/MS/MS method" in Journal of Pharmaceutical and Biomedical Analysis, 146 (2017):48-52, https://doi.org/10.1016/j.jpba.2017.08.017 . .