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Simultaneous Determination of 16 Illegally Added Drugs in Capsule Dietary Supplements Using a QuEChERS Method and HPLC–MS/MS

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Abstract

A simple and rapid method based on the QuEChERS (quick, easy, cheap, effective, rugged, and safe) pretreatment and HPLC–MS/MS (high performance liquid chromatography–tandem mass spectrometry) system was successfully developed and validated for the analysis of 16 illegally added chemical drugs in capsule dietary supplements for weight-loss and lipid reduction. Samples were extracted with acetonitrile solution containing 1% formic acid. Then 500 mg mixed anhydrous magnesium sulfate and sodium chloride (1:1; m/m) were used for salting out, and 100 mg PSA adsorbents were used for purification. 16 analytes rendered good linearity in the range of 0.025–20 μg/g. The limits of detection (LOD) and limits of quantitation (LOQ) ranged from 0.3 to 20 ng/g and 1 to 50 ng/g, respectively. All the linear correlation coefficients were greater than 0.9942. The accuracy values of 16 analytes were between 80.21 and 118.35%, and the stability expressed by relative standard deviations (RSDs) were < 11.06% within three adding levels. Finally, fluoxetine was detected in 2 batch samples by the method. This method is simple, fast, practical and suitable for rapid detection of illegally added drugs in dietary supplements for weight loss and fat reduction. It also provides more powerful technical supports for the supervision of dietary supplements safety and can be used as an analytical method for the detection of such illegally added substances.

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Acknowledgements

This work was supported by the Natural Science Foundation of Hebei Province (H2019329002) and the Hebei Provincial Key Research and Development Program (19275505D, 20327122D, 21327115D). The authors would like to thank all the reviewers who participated in the review for its assistance during the preparation of this manuscript.

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Authors and Affiliations

  1. College of Food and Biology, Hebei University of Science and Technology, Shijiazhuang, 050018, China

    Jinmei Gao & Wenhui Gao

  2. Hebei Institute for Drug and Medical Device Control, Shijiazhuang, 050299, China

    Chunyan Ma, Qiong Duan & Hui Li

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  1. Jinmei Gao
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  2. Chunyan Ma
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Correspondence to Wenhui Gao or Hui Li.

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Gao, J., Ma, C., Duan, Q. et al. Simultaneous Determination of 16 Illegally Added Drugs in Capsule Dietary Supplements Using a QuEChERS Method and HPLC–MS/MS. Chromatographia 84, 1009–1023 (2021). https://doi.org/10.1007/s10337-021-04087-y

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  • DOI: https://doi.org/10.1007/s10337-021-04087-y

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