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In order to obtain comprehensive quality evaluation of one traditional Chinese patent medicine of Mailuoning oral liquid (MLN), one smart strategy combined by fingerprint, qualitative and quantitative analyses were carried out in this study. Firstly, the fingerprints of MLN were established by HPLC-UV and HPLC-ELSD, and explained the similarity of twenty-seven batches of MLN by similarity analysis (SA). Secondly, qualitative analysis was performed by high performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (HPLC-QTOF-MS/MS). A total of 60 compounds were identified or tentatively identified based on chemical standards and fragmentation information. Finally, the quantitative method based on UPLC combined with triple quadrupole mass spectrometry (UPLC-QqQ-MS/MS) was developed for the simultaneous determination of 40 target compounds. The results showed that MLN samples of different productive year were clearly discriminated and eight compounds (5-hydroxymethyl-2-furaldehyde, neochlorogenic acid, loganic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, isoacteoside, angoroside C) were selected as differential markers for MLN. In a word, this strategy including fingerprint, identification of chemical composition and multiple-component quantification could be well applied to modern quality evaluation of MLN, which could be valuable for the further quality control of more other traditional Chinese patent medicines., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023. Published by Elsevier B.V.)

Toxic alkaloids are typically found in herbal medicines and have strong pharmacological effects and a broad therapeutic spectrum. On the other hand, toxic alkaloids exert toxicological activities in vivo; as such they have a narrow therapeutic window and can induce poisoning due to incorrect dose or misuse. In this view, there is an urgent need to develop a rapid and sensitive assay to detect these toxic alkaloids. This study developed a method for determining five common toxic alkaloids in blood, including brucine, strychnine, aconitine, mesaconitine, and hypaconitine using ultra-high liquid chromatography-tandem quadrupole/linear ion trap mass spectrometry (QTRAP UPLC-MS/MS). The analytes in this investigation were extracted with ether and detected using multiple reaction monitoring (MRM)-information-dependent acquisition (IDA)-enhanced product ion (EPI) scanning modes. SKF 525A served as the internal standard (IS). The approach demonstrated excellent linearity, with a correlation coefficient (R) > 0.9964, and satisfactory sensitivity, with the limit of detection (LOD) of 0.31 ∼ 3.26 ng/mL and a limit of quantification (LOQ) of 1.13 ∼ 11.52 ng/mL. The extraction recovery (ER) was 78.8 ∼ 116.2%, the matrix effect (ME) was -12.3 ∼ 21.2%, and the method accuracy was 0.8 ∼ 12.8%. In addition, the intra-day precision and the inter-day precision (RSD) were 0.7% ∼ 7.4% and 0.4% ∼ 13.5%, respectively. The developed approach is sensitive and efficient, and offer significant application prospect in clinical monitoring and forensic detection of poisoning., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Introduction: Aurantii Fructus Immaturus (Zhishi in Chinese) is the dried young fruit of Citrus aurantium L. (CA) and its cultivated varieties or Citrus sinensis Osbeck (CS). The content of flavonoids in different varieties of Zhishi may be significantly different. However, there is confusion about the botanical origin of Zhishi, and there is no reliable and systematic method to control Zhishi quality., Objectives: We aimed to establish an ultrahigh-performance liquid chromatography method coupled with diode-array detection and high-resolution tandem mass spectrometry (UPLC-DAD-HRMS/MS) for the quantitative analysis of 10 flavonoids in Zhishi that could be used for quality control and botanical origin identification., Methodology: A UPLC-DAD-HRMS/MS method was established for simultaneous identification and quantification of 10 flavonoids. Separation was performed on a Waters Acquity UPLC HSS T3 column (100 mm × 2.1 mm, 1.8 μm) with 0.1% formic acid and acetonitrile as mobile phase under gradient elution. MS was performed in positive and negative ionisation modes. The flavonoids in 41 batches were isolated and quantified. Zhishi of different botanical origins were identified by chemometrics., Results: The results showed that the established method for the determination of 10 components was reliable and accurate. Chemometrics could be used to distinguish Zhishi of different botanical origins. There were significant differences in the contents of 10 flavonoids in samples of different botanical origins., Conclusions: The quantitative analysis method in this study can be used to accurately determine the content of 10 flavonoids and provide a chemical basis for quality control and botanical origin identification of Zhishi., (© 2022 John Wiley & Sons, Ltd.)

Edible bird's nest (EBN) is an expensive health food. There are many adulterants in the market. It remains challenging to discriminate EBN from its adulterants due to a lack of high-specificity markers. Besides, the current markers are confined to soluble fraction of EBN. Here, both soluble and insoluble fractions were analyzed by LC-QTOF-MS/MS. A total of 26 high-specificity peptides that were specific to EBN were selected as qualitative authentication markers. Among them, 10 markers can discriminate EBN from common adulterants, 13 markers discriminate white EBN from grass EBN/common adulterants, and 3 markers discriminate grass EBN from white EBN/common adulterants. Three of them, which showed high signal abundance (Peak area ≥ 10 6 ) and satisfactory linearity ( R 2 ≥ 0.995) with EBN references, were selected as the assay marker; and their peptide sequences were confidently identified by searching database/de novo sequencing. Based on these markers, a qualitative and quantitative analytical method was successfully developed and well-validated in terms of linearity, precision, repeatability, and accuracy. The method was subsequently applied to detect EBN products on the market. The results indicated that more than half of EBN products were not consistent with what the merchants claimed.

Vortioxetine (VOR) is a new antidepressant drug used to treat major depressive disorder. In this work, a novel, simple, rapid, accurate, precise, selective, stability-indicating, and fully validated high-performance liquid chromatography method with diode array detection (HPLC-DAD) was developed to determine VOR in bulk and pharmaceutical formulations. A Polar-RP column was used, with a mobile phase consisting of acetonitrile (ACN), methanol (MeOH), acetate buffer pH 3.5, and addition of diethylamine (DEA) in the isocratic elution mode. Assessing the stability of the VOR is fundamental to guarantee the efficacy, safety, and quality of drug products. In this study, the VOR active pharmaceutical ingredient (API) and tablets were subjected to a detailed study of forced degradation, using several degrading agents (acid, alkaline, water, heat, light, and oxidation agents). The developed HPLC-DAD method allows the collection of all the essential data to determine degradation kinetics. It was found that the decomposition of vortioxetine is fragile towards oxidative conditions and photolysis, yielding the first-order and second-order kinetic reaction in the above stress conditions, respectively. The degradation products (DPs) were identified by the high-resolution liquid chromatography coupled with electrospray ionization-quadrupole-time of flight-mass spectrometry (LC-ESI-QTOF-MS) method. The HPLC-DAD method was successfully applied for the quantification of VOR in tablets. Additionally, in silico toxicity prediction of the DPs was performed.

There have been few comprehensive studies on the holistic chemical composition of Spatholobi Caulis (SC) and consequently, the information is lacking for the in-depth study of the major constituents. SC is a kind of widely used traditional Chinese medicine with its xylem and phloem alternately arranged in 3-10 rings, but the relationship of phloem ring number and the quality remains unclear. In this study, the characterization of the major constituents in SC was analyzed by ultra-fast liquid chromatography coupled with triple quadrupole-time of flight tandem mass spectrometry (UFLC-Triple TOF-MS/MS), and the content of 19 flavonoids in SC with different phloem ring numbers was simultaneously determined by ultra-fast liquid chromatography coupled with triple quadrupole-linear ion trap tandem mass spectrometry (UFLC-QTRAP-MS/MS). Correlation analysis was performed to evaluate the quality of SC with different phloem ring numbers according to the content of 19 flavonoids. Results showed that 50 constituents in SC were identified and the fragmentation pathways of different types of compounds were preliminarily deduced by the fragmentation behavior of the 50 constituents. In addition, the content of flavonoids increased with phloem ring number, which demonstrated that the content of flavonoids in SC was positively correlated with the number of phloem rings. Our research will contribute to the variety identification and quality evaluation of SC, and provide a scientific basis for evaluating the quality of medicinal materials based on its appearance and characteristics., Competing Interests: Declaration of Competing Interest The authors report no declarations of interest., (Copyright © 2020 Elsevier B.V. All rights reserved.)

An analytical program for multiclass, multiresidue residue analysis to qualitatively and quantitatively determine veterinary drug compounds in game meats by LC-MS/MS has been developed and validated. The method was validated for the analysis of muscle from bison, deer, elk, and rabbit to test for 112 veterinary drug residues from the following drug classes: β-agonists, anthelmintics, anti-inflammatory drugs, corticosteroids, fluoroquinolones, β-lactams, macrolides, nitroimidazoles, phenicols, polypeptides, sulfonamides, tetracyclines, thyreostats, and tranquilizers. Muscle was extracted using a simple and quick procedure based on a solvent extraction with 80% ACN/water and sample cleanup with dispersive solid-phase extraction. The compounds of interest were separated using a Waters HSS T3 column and detected by tandem mass spectrometry with rapid polarity switching to detect both negatively and positively charged ions in a single run. Recoveries were calculated using extracted matrix-matched calibration curves for each type of matrix. The average accuracy of fortified compounds ranged from 95.6 to 101% at the target quantitative validation level in the four matrices. The method was also validated as a qualitative screening method where all sample responses were compared with a single extracted matrix-matched calibrant at the target testing level (5 or 25 ng/g). Samples demonstrating a presumptive positive above the threshold value were re-extracted and analyzed with a five-point matrix-matching extracted calibration curve. Since the beginning of this survey program, 360 samples have been analyzed for veterinary drug residues in game meats. Antibiotic or tranquilizer residues have been identified in deer (chlortetracycline, haloperidol, and tulathromycin) and rabbit (sulfadiazine).

Introduction: Jian-Pi-Yi-Shen pill (JPYSP) is a Chinese medicine formula developed for the treatment of anaemic patients with chronic kidney disease (CKD)., Objective: To investigate the chemical profile of JPYSP in the treatment of renal anaemia., Methods: A method coupling ultra-performance liquid chromatography with quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MS/MS) was established to characterise the chemical constituents present in JPYSP. Subsequently, a high-performance liquid chromatography method coupled with triple-quadrupole tandem mass spectrometry (HPLC-QQQ-MS/MS) was developed to quantify the major constituents from the identified compounds related to the treatment of CKD and anaemia., Results: A total of 71 compounds were tentatively identified from JPYSP, including saponins, flavonoids, sesquiterpenoids, coumarins, phenylpropanoids, anthranones, anthraquinones, tannins, phenolic acids and others. Amongst them, 12 compounds (i.e. astragaloside IV, calycosin, calycosin 7-O-glucoside, salvianolic acid A, rosmarinic acid, rhein, liquiritin, formononetin, atractylenolide I, dioscin, tanshinone IIA, and acteoside) were further quantified simultaneously by HPLC-QQQ-MS/MS., Conclusion: The newly developed approach is suitable for the chemical profiling analysis and quality control of JPYSP, and could lead to additional pharmacodynamic studies involving the components of JPYSP., (© 2020 John Wiley & Sons, Ltd.)

Meiguihua oral solution (MOS), a classical Chinese medicinal formula, was approved by the China Food and Drug Administration for production. However, the quality evaluation of MOS has not been reported. In this present study, qualitative and quantitative analysis of MOS were conducted by ultra high performance liquid chromatography coupled to quadrupole-orbitrap high resolution mass spectrometry (UHPLC-Q-orbitrap-HRMS) and high performance liquid chromatography-tri-quadrupole linear ion trap mass spectrometry (HPLC-tri-Q-LIT-MS). Totally 46 phenolic compounds (21 flavonoids and 25 tannins) were identified in the MOS, among them 14 polyphenols were not reported in raw plant materials of MOS. The simultaneous quantification of ten compounds including gallic acid, quercetin-3-O-sophoroside, ellagic acid, sophoraflavonoloside, hyperoside, isoquercitrin, avicularin, astragalin, quercitrin and juglanin, which were completed in 16 min in the negative electrospray ionization (ESI) mode under multiple reaction monitoring (MRM) method. Linearity was reached fine determination coefficient (r 2  > 0.9995). Precisions, repeatability, stability (inter-day and intra-day), and recovery were validated and the relative standard deviations (RSD) were less than 2.9%, 4.7%, 3.6% and 1.79%, respectively. This result proved the high sensitivity and efficiency of the method. The quantitative and qualitative analysis of MOS would provide the substantial basis for further quality control and medicinal values., (Copyright © 2020 Elsevier B.V. All rights reserved.)

Radix Dipsaci (RD), the dried root of Dipsacus asper, is used in traditional Chinese medicine as a remedy for bone fractures, traumatic hematoma, threatened abortion, and uterine bleeding. A novel ultra high-performance liquid chromatography coupled with quadrupole-time-of-flight tanderm mass spectrometry (UHPLC-Q-TOF/MS) approach was performed to rapidly characterize the chemical constituents of RD. Consequently, 21 compounds, including 12 iridoid glycosides (IGs), 4 furofuran lignans (FLs), and 5 phenolic acids (PAs) were discovered and identified from RD. Among these compounds, 3 IGs were previously unreported. Furthermore, a rapid and reliable UHPLC-DAD-based method was developed. The linearity (R 2  > 0.999), repeatability (RSDs < 3.0%), intra-day and inter-day precision (RSDs < 1.6%), recovery (98.9%-102.5%), limits of detection (0.2-2.75 ng), and limits of quantification (0.75-8.5 ng) of the method was validated. The method was successfully applied for the simultaneous determination of 11 compounds in 20 batches of RD collected from various geographical regions in China. Different RD samples exhibited significantly varied contents of 11 analytes, among which IGs and PAs are abundant compounds that could be used as suitable quality markers for RD. The present study provided a useful approach for comprehensively evaluating the chemical composition and quality of RD., (Copyright © 2018 Elsevier B.V. All rights reserved.)

Viscum coloratum is a perennial evergreen, semi-parasitic plant. It is generally used for treating cardiovascular diseases, cancer, hepatitis and hemorrhage. In this study, reliable methods were developed for the qualitative and quantitative analysis of the common constituents in Viscum coloratum and its corresponding host. In the rapid qualitative analysis, a method of ultra-high performance liquid chromatography and quadrupole time-of-flight tandem mass spectrometry was established for identification of the same compounds. Based on the retention times, accurate mass measurement and previous literatures, 23 components were clearly identified by comparison with reference substances. In the quantitative analysis, a method for Viscum coloratum and its corresponding host was developed by ultra-high performance liquid chromatography with triple quadrupole mass spectrometry. 13 common compounds of viscum coloratum and host plants from 19 batches were analyzed with a good linearity (r 2 ≥0.9991), intra-day precision (RSD≤3.24%), inter-day precision (RSD≤3.31%), repeatability (RSD≤2.43%), stability (RSD≤2.63%), and recovery (98.2-102.4%). The overall limits of quantification were less than 5.0ng/mL. The results indicated that these effective and comprehensive methods can be applicable to simultaneous qualitative and quantitative analysis of these common compounds presented in Viscum coloratum and corresponding host plants., (Copyright © 2017 Elsevier B.V. All rights reserved.)

In this work, a sensitive and efficient method was established and validated for qualitative and quantitative analysis of major bioactive constituents in Dazhu Hongjingtian capsule by liquid chromatography tandem mass spectrometry. A total of 32 compounds were tentatively identified using ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry. Furthermore, 12 constituents, namely gallic acid, 3,4-dihydroxybenzoic acid, salidroside, p-coumaric acid-4-O-β-d-glucopyranoside, bergeninum, 4-hydroxybenzoic acid, 4-hydroxyphenylacetic acid, syringate, 6''-O-galloylsalidroside, rhodiosin, rhodionin and kaempferol-7-O-α-l-rhamnoside, were simultaneously quantified by the developed ultra-performance liquid chromatography coupled with a triple quadrupole mass spectrometry method in 9 min. All of them were analyzed on an Agilent ZorBax SB-C 18 column (3.0 × 100 mm, 1.8 μm) with linear gradient elution of methanol-0.1% formic acid water. The proposed method was applied to analyze three batches of samples with acceptable linearity (R, 0.9979-0.9997), precision (RSD, 1.3-4.7%), repeatability (RSD, 1.7-4.9%), stability (RSD, 2.2-4.9%) and recovery (RSD, 0.6-4.4%) of the 12 compounds. As a result, the analytical method possessing high throughput and sensitivity is suitable for the quality control of Dazhu Hongjingtian capsule., (Copyright © 2016 John Wiley & Sons, Ltd.)

Highlights • A sensitive and efficient method was established and validated for qualitative and quantitative analysis. • 52 compounds were tentatively identified using UHPLC–ESI–QTOF–MS. • 5 compounds were quantified using UHPLC–ESI–QQQ–MS/MS. • 3 batches samples were analyzed by the proposed method. Abstract A sensitive and efficient method was established and validated for qualitative and quantitative analysis on the chemical constituents in Orthosiphon stamineus Benth. (O. stamineus) using ultra high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry. Based on the retention time and MS spectra, 61 compounds were detected by using ultra high-performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry. 52 chemical structures in the O. stamineus extracts including 26 phenolic acids, 11 flavonoids, 6 diterpenoids, 4 fatty acids and 5 tanshinones were tentatively identified without the time-consuming process of isolation. Moreover, five chemical constituents (Danshensu, Caffeic acid, Rosmarinic acid, Sinensetin and Eupatorin) were quantified in three different batches of O. stamineus samples by the developed ultra high-performance liquid chromatography coupled with electrospray ionization triple-quadrupole mass spectrometry method in 10 min. The method validation of the five compounds was performed with acceptable linearity (R2, 0.9930–0.9997), precision (RSD, 1.87–10.36%), repeatability (RSD, 0.59–4.87%) and recovery (105.30–110.53%, RSD ≤ 13.90%). [ABSTRACT FROM AUTHOR]

In the present work, direct analysis of real time ionization combined with multi-stage tandem mass spectrometry (DART-MS) was used to investigate the metabolic profile of aconite alkaloids in rat intestinal bacteria. A total of 36 metabolites from three aconite alkaloids were identified by using DART-MS, and the feasibility of quantitative analysis of these analytes was examined. Key parameters of the DART ion source, such as helium gas temperature and pressure, the source-to-MS distance, and the speed of the autosampler, were optimized to achieve high sensitivity, enhance reproducibility, and reduce the occurrence of fragmentation. The instrument analysis time for one sample can be less than 10 s for this method. Compared with ESI-MS and UPLC-MS, the DART-MS is more efficient for directly detecting metabolic samples, and has the advantage of being a simple, high-speed, high-throughput method. [Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]