Targeted and nontargeted screening and identification of 50 antihypertensive adulterants in dietary supplements and herbal medicines using quadrupole–orbitrap high resolution mass spectrometry with compound database

Abstract

In the present work, a novel database of drug compounds and a rapid screening method based on ultra‐high performance liquid chromatography coupled to high resolution orbitrap mass spectrometry were developed and applied in the screening and identification of targeted and nontargeted antihypertensive adulterants in dietary supplements and herbal medicines. The established screening database includes retention time, exact mass, fragments, isotopic pattern, and MS2 spectra library of the target compounds and thus provides automated search and identification of the targets with a single injection. The nontargeted compounds in the samples are identified through the full MS scan and MS2 data by using the Chemspider database and the data analysis in XCalibur, MassFrontier and TraceFinder software. In addition, this method possesses excellent quantitative capacity. The novel approach was applied to 65 batches of samples that are claimed as “all‐natural” products having the antihypertensive function, among which nine batches were found to be positive. Multiple targeted and nontargeted antihypertensive adulterants were detected at levels ranging from 2.8 to 27.9 mg/g. The novel database and screening method demonstrated herein will be promising and powerful tools for rapid screening of antihypertensive adulterants in dietary supplements and herbal medicines.

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

“…Overall validation results were summarized in Tables 1 and 2. In this study, calculated LODs for 92 targeted compounds were comparable with previously reported analytical methods using UHPLC-high resolution MS [41][42][43]. The previously reported methods provided LOD ranges within 0.3-2 ng/g, 0.01-0.04 µg/g, and 0.12-1.50 µg/mL, for 13 weight-loss drugs, 50 antihypertensive adulterants, and 20 antigout and anti-osteoporosis drugs, respectively.…”

“…Under the optimized conditions, LODs ranged from 0.1 to 16 ng/g. Furthermore, most substances adulterated in illegal drugs and supplements were found at mg/g levels [41][42][43][44]. Considering the concentration levels of detected adulterants in previous studies, this method enabled sensitive detection for screening of 92 illegal adulterants.…”

Characterization of chemical constituents in Shuanghuanglian oral dosage forms by ultra‐high performance liquid chromatography coupled with time‐of‐flight mass spectrometry

“…The combination of targeted and untargeted identification strategies has been successfully applied to the identifi-cation and characterization of TCM components many times. Hence, similar strategies have been employed in the present study [19][20][21]. Compounds contained in SHL preparations were searched in Chemspider, PubMed, Elsevier Science Direct, and Massbank databases.…”

Chemical profiling of Honghua Xiaoyao tablet and simultaneous determination of its quality markers by liquid chromatography–tandem mass spectrometry combined with chemometrics methods

“…Ultra-high/high-performance liquid chromatography technique (UH/HPLC), combined with highresolution quadrupole/time-of-flight mass spectrometry (Q-TOF/MS) or triple quadrupole mass spectrometry (QQQ/MS), has been not only used as an effective and powerful technique for qualitative analysis of almost all of the components, but also internationally acknowledged for the quality evaluation of TCM, TCM formula, or their related products [13,14]. The former technique is an efficient tool for high-throughput screening of compounds due to the 2D acquisitions modes, including data-independent acquisition (MS E ) and fast data-directed analysis (Fast DDA).…”