Reliable screening and confirmation of 156 multi-class illegal adulterants in dietary supplements based on extracted common ion chromatograms by ultra-high-performance liquid chromatography-quadrupole/time of flight-mass spectrometry

Kim, Eun Hye; Seo, Hee Seung; Ki, Nam Yong; Park, Na-Hyun; Lee, Wonwoong; Ah, Jung; Park, Sung-Kwan; Lee, Ji Hyun; Moon, Bongjin; Oh, Han Bin; Hong, Jongki

doi:10.1016/j.chroma.2017.02.032

Cited by 33 publications

(19 citation statements)

References 32 publications

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“…In this study, a UHPLC-Q/TOF-MS method was developed to determine multi-class 92 illegal adulterants. Conditions for LC separation and MS detection were modified slightly based on our previous studies [16,17]. To efficiently separate 92 illegal adulterants, several LC conditions (such as three analytical columns (HSS T3, UPLC BEH C18, and biphenyl with same dimension (150 × 2.1 mm, 1.7 μm)), mobile phase flow rates (250, 300, 350, and 400 μL/min), and column temperatures (20,30,40, and 50 °C)) were evaluated.…”

Section: Analysis Of 92 Illegal Adulterants By Uhplc-q/tof-msmentioning

confidence: 99%

“…To supervise and prevent illegal adulterations in dietary supplements, numerous screening methods have been developed to effectively detect a wide range of illegal adulterants in various supplement formulations. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) and quadrupole/time of flight (Q/TOF) MS methods have most often been used for screening of a wide range of unauthorized drugs in various supplements due to their high sensitivity, selectivity, and convenience [14][15][16][17]. LC-MS methods with aid from multiple reaction monitoring (MRM), extracted ion chromatogram (EIC), extracted common ion chromatogram (ECIC), and neutral loss scan (NLS) modes have all facilitated multi-class drug screening for various types of supplement.…”

Section: Introductionmentioning

confidence: 99%

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Efficient Matrix Cleanup of Soft-Gel-Type Dietary Supplements for Rapid Screening of 92 Illegal Adulterants Using EMR-Lipid dSPE and UHPLC-Q/TOF-MS

et al. 2021

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An efficient matrix cleanup method was developed for the rapid screening of 92 illegal adulterants (25 erectile dysfunction drugs, 15 steroids, seven anabolic steroids, 12 antihistamines, 12 nonsteroidal anti-inflammatory drugs (NSAIDs), four diuretics, and 17 weight-loss drugs) in soft-gel-type supplements by ultra-high performance liquid chromatography-quadrupole/time of flight-mass spectrometry (UHPLC-Q/TOF-MS). As representative green chemistry methods, three sample preparation methods (dispersive liquid-liquid microextraction (DLLME), “quick, easy, cheap, effective, rugged, and safe” dispersive solid-phase extraction (QuEChERS-dSPE), and enhanced matrix removal-lipid (EMR-Lipid) dSPE) were evaluated for matrix removal efficiency, recovery rate, and matrix effect. In this study, EMR-Lipid dSPE was shown to effectively remove complicated matrix contents in soft-gels, compared to DLLME and QuEChERS-dSPE. For the rapid screening of a wide range of adulterants, extracted common ion chromatogram (ECIC) and neutral loss scan (NLS) based on specific common MS/MS fragments were applied to randomly collected soft-gel-type dietary supplement samples using UHPLC-Q/TOF-MS. Both ECICs and NLSs enabled rapid and simple screening of multi-class adulterants and could be an alternative to the multiple reaction monitoring (MRM) method. The developed method was validated in terms of limit of detection (LOD), precision, accuracy, recovery, and matrix effects. The range of LODs was 0.1–16 ng/g. The overall precision values were within 0.09–14.65%. The accuracy ranged from 81.6% to 116.6%. The recoveries and matrix effects of 92 illegal adulterants ranged within 16.9–119.4% and 69.8–114.8%, respectively. The established method was successfully applied to screen and identify 92 illegal adulterants in soft-gels. This method can be a promising tool for the high-throughput screening of various adulterants in dietary supplements and could be used as a more environmentally friendly routine analytical method for screening dietary supplements illegally adulterated with multi-class drug substances.

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Section: Analysis Of 92 Illegal Adulterants By Uhplc-q/tof-msmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Efficient Matrix Cleanup of Soft-Gel-Type Dietary Supplements for Rapid Screening of 92 Illegal Adulterants Using EMR-Lipid dSPE and UHPLC-Q/TOF-MS

et al. 2021

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“…[13][14][15][16] More commonly, liquid chromatography (LC) coupled with tandem mass spectrometry (MS/MS) has proven to be invaluable in the analysis of PDE5 inhibitors. 17,18 However, LC-MS/MS, in general, demands higher operational and maintenance costs with limited sample throughput. It also requires experienced users to operate the analytical instrument and interpret the MS data.…”

Section: Introductionmentioning

confidence: 99%

“…At present, several analytical methods have been utilised to determine PDE5 inhibitors in various matrices 13–16 . More commonly, liquid chromatography (LC) coupled with tandem mass spectrometry (MS/MS) has proven to be invaluable in the analysis of PDE5 inhibitors 17,18 . However, LC–MS/MS, in general, demands higher operational and maintenance costs with limited sample throughput.…”

Section: Introductionmentioning

confidence: 99%

Fluorescence polarisation for high‐throughput screening of adulterated food products via phosphodiesterase 5 inhibition assay

Yusop

Xiao

2020

Drug Testing and Analysis

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“…HPLC equipped with ESI-MS/MS is a well-established and widespread technique for the analysis of various compounds illegally used to adulterants of sexual enhancement and weight loss compounds in dietary supplements [ 6 , 7 , 8 ]. Due to the increase in the adulteration of illegal compounds in dietary supplements, several analytical methods have been previously reported using liquid chromatography tandem mass spectrometry (LC-MS/MS) [ 9 , 10 , 11 , 12 ]. In addition, the multi-class analytical method using LC–MS/MS is widely applied for reliable quantitation and confirmation of illicit compounds [ 13 , 14 ].…”

Section: Introductionmentioning

confidence: 99%

Multi-Class Determination of 64 Illicit Compounds in Dietary Supplements Using Liquid Chromatography–Tandem Mass Spectrometry

et al. 2020

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In this work, liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed and validated for screening and confirmation of 64 illicit compounds in dietary supplements. The target compounds were illegally used pharmaceutical drugs, prohibited compounds, and not authorized ingredients for different therapeutics (sexual enhancement, weight loss, muscular strengthening, and relaxing products). The validation procedure was performed to evaluate selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision according to the Association of Official Analytical Chemists guidelines. The linearity was >0.98 in the range of 0.5–200 µg L−1. The LOQs were in the range 1–10 µg kg−1 for all target compounds. The accuracy (expressed as recovery) was 78.5–114%. The precision (expressed as the relative standard deviation) was below 9.15%. The developed method was applied for the determination of illicit compounds in dietary supplements collected from websites. As a result, the total detection rate was 13.5% (27 samples detected in 200 samples). The concentrations of detected samples ranged from 0.51 to 226 mg g−1. The proposed methodology is suitable for monitoring the adulteration of illicit compounds in dietary supplements.

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Reliable screening and confirmation of 156 multi-class illegal adulterants in dietary supplements based on extracted common ion chromatograms by ultra-high-performance liquid chromatography-quadrupole/time of flight-mass spectrometry

Cited by 33 publications

References 32 publications

Efficient Matrix Cleanup of Soft-Gel-Type Dietary Supplements for Rapid Screening of 92 Illegal Adulterants Using EMR-Lipid dSPE and UHPLC-Q/TOF-MS

Efficient Matrix Cleanup of Soft-Gel-Type Dietary Supplements for Rapid Screening of 92 Illegal Adulterants Using EMR-Lipid dSPE and UHPLC-Q/TOF-MS

Fluorescence polarisation for high‐throughput screening of adulterated food products via phosphodiesterase 5 inhibition assay

Multi-Class Determination of 64 Illicit Compounds in Dietary Supplements Using Liquid Chromatography–Tandem Mass Spectrometry

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