A hierarchical screening method for detection of illegal adulterants in Fur seal ginseng pills by profiling analysis of HPLC multi‐dimensional fingerprints

Abstract

A novel method for hierarchical screening of illegal adulterants in Fur seal ginseng pills products was developed by multi-dimensional fingerprint profiling analysis. Fingerprint feature of the samples was acquired by high-performance liquid chromatography analysis of 11 batches of samples with diode array detector and fluorescence detector, and then potential illegal adulterants including phosphodiesterase type-5 inhibitors, androgens, α receptor antagonists and yohimbine, were further separated at multiple wavelengths to reduce or remove interferences from sample matrix for highlight their chromatographic characteristics. Accordingly, a hierarchical screening strategy was designed by first-order and second-order fingerprints combined with spectral examination to achieve high accuracy and reliability. The method was successfully applied to screening of illegal adulterants in real samples, and it also exhibited good quantification performance through validation tests. From 16 batches of samples, three suspected samples were confirmed to be positive, containing 9.37μg/g of testosterone, 18.8 μg/g of tadalafil, and 48.5 μg/g of sildenafil, respectively. The recoveries and relative standard deviations were in the range of 83.6-103.1% and 4.2-6.8%, respectively. The proposed method provided a simple, efficient and promising alternative to monitoring functional foods. K E Y W O R D S functional foods, Fur seal ginseng pills, hierarchical screening, illegal adulterants, multi-dimensional fingerprints, traditional Chinese medicine J Sep Sci 2019;42:1509-1519.

Interpol Review of Drug Analysis 2019-2022

“…2019 Rapid detection of adulteration of dehydroepiandrosterone in slimming products by competitive indirect enzyme-linked immunosorbent assay and lateral flow immunochromatography [ 832 ]; screening method for detection of illegal adulterants in ginseng pills by profiling analysis of HPLC multi-dimensional fingerprints [ 833 ]; 2020 identification of tert-butyl-4-anilinopiperidine-1-carboxylate (4-anilinopiperdine-t-BOC or 4-AP-t-BOC) in seized falsified ‘Xanax’ tablets and suspected heroin seizures [ 834 ]; 20 herbal mixtures containing Cumyl-PEGACLONE were quantitatively analyzed by HPLC-DAD after an initial screening by gas chromatography mass spectrometry [ 835 ]; simultaneous and reliable determination of 20 pharmaceutical compounds in adulterated health food products using liquid chromatography with electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) and liquid chromatography with quadrupole-time-of-flight mass spectrometry (LC-QTOF-MS) [ 836 ]; MALDI-MS method for analysis of illegal drugs and doped substances added in supplements [ 837 ]; 2021 voltammetric method for analyzing weight loss products adulterated amphetamine [ 838 ]; development and validation of an HPLC-MS/MS system for the analysis of 16 chemical drugs illegally added to dietary supplements for weight-loss in a capsule form [ 839 ]; quantification of pharmaceuticals or prescription medications (fluoxetine, phenolphthalein, and sibutramine illegally added to herbal weight loss supplements by RP-HPLC-MS/MS [ 840 ]; IMS qualitiative screening method for illicit additives (ibuprofen, nitrazepam, nitrendipine, indomethacin, phenobarbital, sibutramine, diclofenac sodium, diazepam, estazolam, melatonin, phenolphthalein, prednisone acetate, betamethasone, metformin HCl, glibenclamide, and tadalafil) in herbal pharmaceuticals and health foods with quantification by HPLC [ 841 ]; UPLC-PDA and LC/EIS-MS/MS methods for simultaneously screening for 25 anti-hyperlipidemic substances illegally added to dietary supplements [ 842 ]; HPLC-DAD method for the identification and quantification of sexual stimulants and anabolic steroids in the adulterated dietary supplements [ 843 ]; MALDI-MS method for the analysis of illegally added and doped substances added to medicines or food [ 837 ]; 2022 mixed-mode sorbent for SPE of hydrophobic and hydrophilic illegal additives from food sample followed by analysis by RPLC/HILIC-MS/MS [ 844 ]; analytical techniques and metrological principles in studying dietary supplement products and ingredients, particularly medicinal plants and other botanicals [ 845 ]; a membrane-protected micro-SPE method based on molecular imprinting and its application to the determination of local anesthetics illegally added to cosmetics [ 846 ]; application of predicted fragmentation pathways and fragment ion structures with LC-QTOF-MS for the analysis of 15 steroids and 20 selective androgen receptor modulators in dietary supplements [ 847 ]; development of an atmospheric pressure solids analysis probe coupled with single-quadrupole mass spectrometer (A...…”

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