Abstract
An analytical method based on UHPLC-PDA and LC–ESI–MS/MS was developed for the simultaneous and reliable determination of 22 antidepressant and anti-anxiety pharmaceutical compounds in adulterated functional foods. The method was validated in terms of specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), method detection limit (MDL), method quantitation limit (MQL), precision, accuracy, recovery, stability, and matrix effect. For solid and liquid blank samples, the developed method had LOD = 0.10–1.01 μg/mL for UHPLC and 0.01–5.05 ng/mL for LC–ESI–MS/MS, respectively, LOQ = 0.30–3.02 μg/mL and 0.03–15.15 ng/mL, and R2 > 0.999 and R2 > 0.99. Recoveries from spiked blank samples in powder, liquid, tablet, and capsule forms were determined to be 80.13–113.76%. The precision, accuracy, and stability were acceptable, and the matrix effect was insignificant. A total of 118 real samples were successfully analysed using the proposed rapid screening method.
Similar content being viewed by others
Data Availability
The authors confirm that the data supporting the findings of this study are available within the article and its supplementary materials.
References
World Health Organization (2020) Depression. https://www.who.int/news-room/fact-sheets/detail/depression. (Accessed 30 Jan 2020)
Seo YB, Han AL, Shin SR (2019) The association of health related quality of life and depression between obesity in Korean population. J Health Infor Stat 44(2):117–124
American Psychological Association (2000) Anxiety. https://www.apa.org/topics/anxiety. (Accessed 1 Jan 2000)
Sarbacher CA, Halper JT (2019) Connective tissue and age-related diseases. Subcell Biochem 91:281–310
Chinchilla SP, Doherty M, Abhishek A (2019) Gout Activity Score has predictive validity and is sensitive to change: results from the Nottingham Gout Treatment Trial (Phase II). Rheumatology 58:1378–1382
Ministry of Food and Drug Safety (2019) Korean Food Standard Codex. Ministry of Food and Drug Safety; http://www.foodsafetykorea.go.kr/foodcode/01_03.jsp?idx=12. (in Korean) (Accessed 01 Sep 2019)
Kim HS (2016) The popular diet supplementary had detected poison. idomin.com. http://www.idomin.com/news/articleView.html?idxno=521682(in Korean) (Accessed 27 Oct 2016)
US Food and Drug Administration (2016) Public Notification: Adipessum Miracle Slimming Capsules contain hidden drug ingredient. https://www.fda.gov/drugs/medication-health-fraud/public-notification-adipessum-miracle-slimming-capsules-contain-hidden-drug-ingredient. (Accessed 23 Feb 2018)
US Food and Drug Administration (2016) Public Notification: Dream Body Advanced + Acai Weight Loss and Cleanse contains hidden drug ingredients. https://www.fda.gov/drugs/medication-health-fraud/public-notification-dream-body-advanced-acai-weight-loss-cleanse-contains-hidden-drug-ingredients. (Accessed 16 Feb 2018)
Center for Science in the Public Interest (2020) FDA Urged to Protect Consumers from Illegal Sales of Tianeptine. https://cspinet.org/news/fda-urged-protect-consumers-illegal-sales-tianeptine-20200825. (Accessed 25 Aug 2020)
Biesterbos JWH, Sijm DTHM, Dam RV, Mol HGJ (2019) A health risk for consumers: the presence of adulterated food supplements in the Netherlands. Food Addit Contam A 36(9):1273–1288
Kim JY, Park HJ, Kim JW, Lee JH, Heo S, Yoon CY, Cho SY (2015) Development and validation of UPLC and LC-MS/MS methods for the simultaneous determination of anti-obesity drugs in foods and dietary supplements. Arch Pharm Res 39:103–114
Montenarh DB, Wernet MP, Hopf M, Maurer HH, Schmidt PH, Ewald AH (2014) Quantification of 33 antidepressants by LC-MS/MS-comparative validation in whole blood, plasma, and serum. Anal Bioanal Chem 406:5939–5953
Shinozuka T, Terada M, Tanaka E (2006) Solid-phase extraction and analysis of 20 antidepressant drugs in human plasma by LC/MS with SSI method. Forensic Sci Int 162:108–112
Castro AD, Concheiro M, Quintela O, Cruz A, Lopez-Rivadulla M (2008) LC-MS/MS method for the determination of nine antidepressants and some of their main metabolites in oral fluid and plasma study of correlation between venlafaxine concentrations in both matrices. J Pharm Biomed Anal 48:183–193
Castro AD, Fernandez MDMR, Laloup M, Samyn N, Boeck GD, Wood M, Maes V, Lopez-Rivadulla M (2007) High-throughput online solid-phase extraction-liquid chromatography-tandem mass spectrometry method for the simultaneous analysis of 14 antidepressants and their metabolites in plasma. J Chromatogr A 1160(1–2):3–12
Frahnert C, Rao ML, Grasmader K (2003) Analysis of eighteen antidepressants, four atypical antipsychotics and active metabolites in serum by liquid chromatography: a simple tool for therapeutic drug monitoring. J Chromatogr B 794:35–47
Juan H, Zhiling Z, Huande L (2005) Simultaneous determination of fluoxetine, citalopram, paroxetine, venlafaxine in plasma by high performance liquid chromatography-electrospray ionization mass spectrometry (HPLC-MS/ESI). J Chromatogr B 820:35–39
Dunn JD, Gryniewicz-Ruzicka CM, Mans DJ, Mecker-Pogue LC, Kauffman JF, Westenberger NJ, Buhse LF (2012) Qualitative screening for adulterants in weight-loss supplements by ion mobility spectrometry. J Pharm Biomed Anal 71:18–26
Larissa SM, Ana PLM, Diana TM, Carine V, Leandro MDC (2019) An Ultra-High Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometric method for screening and simultaneous determination of anorexic, anxiolytic, antidepressant, diuretic, laxative and stimulant drugs in dietary supplements marketed for weight loss. J Chromatogr Sci 57(6):528–540
Paula P, Manuela JER, Manuela C, Joana SA, Beatriz M, Oliveira PP, Cristina DM (2017) Analysis of pharmaceutical adulterants in plant food supplements by UHPLC-MS/MS. Eur J Pharm Sci 99:219–227
European Medicines Agency (2015) Harmonized tripartite guideline, validation of analytical procedures: text and methodology Q2(R1). International Conference on Harmonization. European Medicines Agency, London
Moschou IC, Dasenaki ME, Thomaidis NS (2019) Ionization study and simultaneous determination of avermectins and milbemycines in fish tissue by LC–ESI–MS/MS. J Chromatogr B 1104:134–140
Dasenaki ME, Thomaidis NS (2015) Multi-residue determination of 115 veterinary drugs and pharmaceutical residues in milk powder, butter, fish tissue and eggs using liquid chromatography–tandem mass spectrometry. Anal Chim Acta 880:103–121
Montenarh D, Hopf A, Warth S, Maurer HH, Schmidt P, Ewald AH (2014) A simple extraction and LC–MS/MS approach for the screening and identification of over 100 analytes in eight different matrices. Drug Test Anal 7(3):214–240
Licata M, Rustichelli C, Palazzoli F, Ferrari A, Baraldi C, Vandelli D, Verri P, Marchesi F, Silingardi E (2016) Hair testing in clinical setting: Simultaneous determination of 50 psychoactive drugs and metabolites in headache patients by LC tandem MS. J Pharm Biomed Anal 126:14–25
Mercolini L, Colliva C, Amore M, Fanali S, Raggi MA (2008) HPLC analysis of the antidepressant trazodone and its main metabolite m-CPP in human plasma. J Pharm Biomed Anal 47:882–887
Park DG, Choi HY, Jang MH, Chang HJ, Woo SH, Yang WY (2018) Simultaneous determination of 18 psychoactive agents and 6 metabolites in plasma using LC-MS/MS and application to actual plasma samples from conscription candidates. Forensic Sci Int 288:283–290
Gaugler SF, Rykl J, Grill M, Cebolla VL (2018) Fully automated drug screening of dried blood spots using online LC–MS/MS analysis. J Appl Bioanal 4(1):7–15
Jettanajit A, Nhujak T (2016) Determination of mycotoxins in brown rice using QuEChERS sample preparation and UHPLC–MS–MS. J Chromatogr Sci 54(5):720–729
Lee JH, Park HN, Choi JY, Kim NS, Park HY, Park SS, Baek SY (2017) Simultaneous analysis by Quadrupole-Orbitrap mass spectrometry and UHPLC–MS/MS for the determination of sedative-hypnotics and sleep inducers in adulterated products. J Sep Sci 40(24):1–12
Kim HJ, Kang JS (2016) Matrix effects: Hurdle for development and validation of bioanalytical LC–MS methods in biological samples analyses. Biodesign 4(2):46–58
Kim NS, Kim JH, Lim NY, Lee JH, Park SS, Kang HI (2020) Simultaneous determination of illegal drug substances in dietary supplements for gout and osteoporosis using ultra-performance liquid chromatography and liquid chromatography-quadrupole-time-of-flight mass spectrometry. J Pharm Biomed Anal 179:1–7
Acknowledgements
This study was supported by a grant (Number: 18181MFDS421) from the Ministry of Food and Drug Safety of Korea in 2019.
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Conflict of Interest
The authors declare that they have no conflict of interest.
Additional information
Publisher's Note
Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
Supplementary Information
Below is the link to the electronic supplementary material.
Rights and permissions
About this article
Cite this article
Kim, N.S., Choi, H.S., Lim, N.Y. et al. Application of Simultaneously Validated UHPLC-PDA and LC–ESI–MS/MS Methods for Determining 22 Antidepressants and Anxiolytics in Food Matrix Samples. Chromatographia 84, 233–247 (2021). https://doi.org/10.1007/s10337-020-04000-z
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10337-020-04000-z