• P-ISSN2233-4203
  • E-ISSN2093-8950

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  • P-ISSN 2233-4203
  • E-ISSN 2093-8950

Simultaneous Determination of 80 Unapproved Compounds using HPLC and LC-MS/MS in Dietary Supplements

Mass Spectrometry Letters, (P)2233-4203; (E)2093-8950
2022, v.13 no.3, pp.58-83
https://doi.org/10.5478/MSL.2022.13.2.58
Kwon Jeongeun (National Institute of Food and Drug Safety Evaluation)
Shin Dasom (National Institute of Food and Drug Safety Evaluation)
Kang Hui-Seung (National Institute of Food and Drug Safety Evaluation)
Suh Junghyuck (National Institute of Food and Drug Safety Evaluation)
Lee Gunyoung (National Institute of Food and Drug Safety Evaluation)
Lee Eunju (National Institute of Food and Drug Safety Evaluation)
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Abstract

We developed analytical methods using high performance chromatography (HPLC) and liquid chromatography tan- dem mass spectrometry (LC-MS/MS) for the simultaneous determination of 80 unapproved compounds in dietary supplements. The target compounds for analysis were unapproved ingredients (e.g., pharmaceuticals) that have potential adverse effects on consumers owing to accidental misuse, overuse, and interaction with other medication in dietary supplement. Two analytical methods were tested to identify the optimal validation results according to AOAC guideline. As a result, limit of quantification (LOQ) was 0.14–0.5 μg mL –1 ; linearity (r 2 ) was ≥ 0.99; accuracy (expressed as recovery) was 78.9–114%; precision (relative standard deviation) was ≤ 4.28% in the HPLC method. In the LC-MS/MS method, LOQ was 0.01–2 ng mL –1 , linearity (r 2 ) was ≥ 0.98, accuracy was 71.7–119%; precision was ≤12.5%. The developed methods were applied to 51 dietary supplements col- lected from 2019 to 2021 through MFDS alert system. Based on our previous monitoring study, major compounds were icariin, sibutramine, yohimbine, sildenafil, tadalafil, sennosides (A, B), cascarosides (A, B, C, D), and phenolphthalein. In this study, we re-analyzed samples of detected compounds, and evaluated the statistical difference using Bland-Altman analysis to compare two analytical approaches between HPLC and LC-MS/MS. These results showed a good agreement between two methods that can be used to monitor the unapproved ingredients in dietary supplements. The developed two methods are complementarily suitable for monitoring the adulteration of 80 unapproved compounds in dietary supplements.

keywords
illicit compounds dietary supplements unapproved ingredients HPLC LC-MS/MS


Submission Date
2022-06-29
Revised Date
2022-09-17
Accepted Date
2022-09-20
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Mass Spectrometry Letters