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Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients

A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: closed (31 July 2023) | Viewed by 25285

Special Issue Editors

Prof. Dr. Angelo Antonio D'Archivio

E-Mail Website
Guest Editor
Department of Physical and Chemical Sciences, University of L’Aquila, Via Vetoio Coppito, 67100 L’Aquila, Italy
Interests: chromatographic analysis; application of chemometrics to data analysis and optimization; quantitative structure-property relationship methodology; food analysis; food traceability
Special Issues, Collections and Topics in MDPI journals
Dr. Alessandra Biancolillo

E-Mail Website
Guest Editor
Department of Physical and Chemical Sciences, University of L’Aquila, Via Vetoio Coppito, 67100 L’Aquila, Italy
Interests: data analysis; chemometrics; food analysis; data-fusion; spectroscopy; classification; variable selection; analytical chemistry
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Collesgues,

In recent years, analytical methodologies have seen exponential advancement; two obvious reasons of this are the development of new instruments and the profitable combination with chemometrics. As a consequence, more and more informative data are commonly available, and refined tools are necessary. The present Special Issue aims to collect new advanced analytical methodologies developed with the intent of characterizing, authenticating, or tracing a class of high-value and hugely investigated products such as food, beverages, natural active ingredients, and pharmaceutical drugs. In light of this, the submission of research works where analytical methods are coupled with chemometrics in order to check the quality and/or inspect foods, pharmaceutical drugs, or natural products is very welcome. Similarly, the submission of reviews providing critic analyses on the most recent tools in this field of research is strongly encouraged.

Prof. Dr. Angelo Antonio D'Archivio
Dr. Alessandra Biancolillo
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Molecules is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2700 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • authentication
  • classification
  • pharmaceutical drugs
  • food
  • quality control
  • natural products
  • geographical origin
  • chemometrics

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Published Papers (17 papers)

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Research

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18 pages, 1722 KiB  
Article
Development and Comparative Evaluation of Two Different Label-Free and Sensitive Fluorescence Platforms for Analysis of Olaparib: A Recently FDA-Approved Drug for the Treatment of Ovarian and Breast Cancer
by Ibrahim A. Darwish and Nasr Y. Khalil
Molecules 2023, 28(18), 6524; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28186524 - 08 Sep 2023
Cited by 1 | Viewed by 881
Abstract
Olaparib (OLA) is a PARP inhibitor drug which has been recently approved by the Food and Drug Administration (FDA) for the treatment of ovarian and breast cancer. A convenient analytical tool for the quantitation of OLA in its dosage form and plasma samples [...] Read more.
Olaparib (OLA) is a PARP inhibitor drug which has been recently approved by the Food and Drug Administration (FDA) for the treatment of ovarian and breast cancer. A convenient analytical tool for the quantitation of OLA in its dosage form and plasma samples was urgently needed. This study describes, for the first time, the development of two different label-free and sensitive fluorescence-based platforms for the pharmaceutical and bioanalysis of OLA. These platforms were microwell-assisted with a fluorescence microplate reader (MW-FLR) and high-performance liquid chromatography with fluorescence detection (HPLC-FD). Both MW-FLR and HPLC-FD employed the native fluorescence of OLA as an analytical signal. The MW-FLR involved measuring the fluorescence signals in 96-well white-opaque plates. The HPLC-FD involved chromatographic separation of OLA and duvelisib (DUV), as an internal standard on a Nucleosil-CN HPLC column (250 mm length × 4.6 mm i.d., 5 µm particle diameter) with a mobile phase composed of acetonitrile: water (25:75, v/v) pumped at a flow rate of 1.7 mL/min. Elution of OLA and DUV was detected using a fluorescence detector. The optimal conditions of both MW-FLR and HPLC-FD were established, and they were validated according to the guidelines of the International Council for Harmonization for the validation of analytical procedures. The linear ranges of MW-FLR and HPLC-FD were 25–1000 and 5–200 ng/mL, respectively, with limits of detection of 15 and 1.7 ng/mL, respectively. The accuracy and precision of both platforms were confirmed as the recovery values were ≥98.2% and the relative standard deviations (RSD) were ≤2.89%. Both methodologies were satisfactorily applied to the quantitation of OLA in its commercial dosage form (Lynparza® tablets) and plasma samples with high accuracy and precision. The greenness of both MW-FLR and HPLC-FD was assessed using two different multiple parameter-based metric tools, and the results proved their greenness and adherence to the requirements of green analytical approaches. Both platforms have simple procedures and acceptable levels of analytical throughput. In conclusion, the proposed MW-FLR and HPLC-FD are valuable tools for routine use in quality control and clinical laboratories for the quantitation of OLA for the purposes of pharmaceutical quality control, pharmacokinetic studies, and bioequivalence testing. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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22 pages, 3783 KiB  
Article
A Pharmacokinetic Study of Sixteen Major Bioactive Components of Jinshui-Huanxian Granules in Pulmonary Fibrosis Model and Control Rats Using Orbitrap Fusion Mass Spectrometry
by Weiwei Zhang, Yan Wan, Shuding Sun, Yang Xie, Di Zhao, Bing Li, Jiansheng Li, Yange Tian and Suxiang Feng
Molecules 2023, 28(18), 6492; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28186492 - 07 Sep 2023
Viewed by 780
Abstract
Jinshui-Huanxian granules (JHGs), a Chinese herbal compound prescription, have shown a therapeutic effect in reducing lung tissue damage, improving the degree of pulmonary fibrosis, replenishing lungs and kidneys, relieving cough and asthma, reducing phlegm, and activating blood circulation. However, these active compounds’ pharmacokinetics [...] Read more.
Jinshui-Huanxian granules (JHGs), a Chinese herbal compound prescription, have shown a therapeutic effect in reducing lung tissue damage, improving the degree of pulmonary fibrosis, replenishing lungs and kidneys, relieving cough and asthma, reducing phlegm, and activating blood circulation. However, these active compounds’ pharmacokinetics and metabolic processes were unclear. This study aimed to compare the pharmacokinetics, reveal the metabolic dynamic changes, and obtain the basic pharmacokinetic parameters of 16 main bioactive compounds after intragastric administration of JHGs in control and pulmonary fibrosis (PF) model rats by using Orbitrap Fusion MS. After administration of JHGs, the rat plasma was collected at different times. Pretreating the plasma sample with methanol and internal standard (IS) solution carbamazepine (CBZ), and it was then applied to a C18 column by setting gradient elution with a mobile phase consisting of methanol 0.1% formic acid aqueous solution. Detection was performed on an electrospray ionization source (ESI), and the scanning mode was SIM. Pharmacokinetic parameters were analyzed according to the different analytes’ concentrations in plasma. The matrix effect was within the range of 79.01–110.90%, the extraction recovery rate was 80.37–102.72%, the intra-day and inter-day precision relative standard deviation (RSD) was less than 7.76%, and the stability was good, which met the requirements of biological sample testing. The method was validated (r ≥ 0.9955) and applied to compare the pharmacokinetic profiles of the control group and PF model group after intragastric administration of the JHGs. The 16 analytes exhibited different pharmacokinetic behaviors in vivo. In the pathological state of the PF model, most of the components were more favorable for metabolism and absorption, and it was more meaningful to study the pharmacokinetics. Above all, this study provided an essential reference for exploring the mechanism of action of JHGs and guided clinical medication as well. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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20 pages, 4180 KiB  
Article
Quality Assessment and Classification of Codonopsis Radix Based on Fingerprints and Chemometrics
by Xuxia Liu, Zhengjun Chen, Xin Wang, Wenrong Luo and Fude Yang
Molecules 2023, 28(13), 5127; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28135127 - 29 Jun 2023
Cited by 2 | Viewed by 1022
Abstract
In China, Codonopsis Radix (CR) is frequently consumed both as food and medicine. Here, a comprehensive strategy based on fingerprinting and chemometric approaches was created to explore the influence of origins, storage time and kneading processing on the quality of CR. Firstly, high-performance [...] Read more.
In China, Codonopsis Radix (CR) is frequently consumed both as food and medicine. Here, a comprehensive strategy based on fingerprinting and chemometric approaches was created to explore the influence of origins, storage time and kneading processing on the quality of CR. Firstly, high-performance liquid chromatography with diode array detection was used to obtain the fingerprints of 35 batches of CR from six different origins and 33 batches of CR from varying storage times or kneading procedures. Secondly, chemometric methods including similarity analysis (SA), principal component analysis (PCA), hierarchical clustering analysis (HCA), and two-way orthogonal partial least square with discriminant analysis (O2PLS—DA) were used to evaluate the differences of chemical components in CR so as to identify its source and reflect its quality. Moreover, 13 and 16 major compounds were identified as marker compounds for the discrimination of CR from different origins, storage time and kneading processing, respectively. Furthermore, the relative content of the marker components and the exact content of Lobetyolin were measured, indicating that the contents of these components vary significantly between various CR samples. Meanwhile, the chemical components of CR were identified using Mass spectrometry. According to the findings of our investigation, the quality of CR from Gansu was the best, followed by Shanxi and then Sichuan. The quality of CR from Chongqing and Guizhou was poor. At the same time, the quality of CR was the best when it was kneaded and stored for 0 years, indicating that the traditional kneading process of CR is of great significance. Conclusively, HPLC fingerprint in conjunction with chemical pattern recognition and component content determination can be employed to differentiate the raw materials of different CR samples. Additionally, it is also a reliable, comprehensive and prospective method for quality control and evaluation of CR. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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14 pages, 4382 KiB  
Article
Application of Band-Selective HSQC NMR in Species Discrimination and Adulteration Identification of Panax Linn
by Congcong Guo, Jiyang Dong, Lingli Deng, Kiankai Cheng, Yue Xu, Haowen Zhu, Anjun Deng, Xia Zhou, Hailin Qin and Yinghong Wang
Molecules 2023, 28(11), 4332; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28114332 - 25 May 2023
Viewed by 1085
Abstract
The quality of Panax Linn products available in the market is threatened by adulteration with different Panax species, such as Panax quinquefolium (PQ), Panax ginseng (PG), and Panax notoginseng (PN). In this paper, we established a 2D [...] Read more.
The quality of Panax Linn products available in the market is threatened by adulteration with different Panax species, such as Panax quinquefolium (PQ), Panax ginseng (PG), and Panax notoginseng (PN). In this paper, we established a 2D band-selective heteronuclear single quantum coherence (bs-HSQC) NMR method to discriminate species and detect adulteration of Panax Linn. The method involves selective excitation of the anomeric carbon resonance region of saponins and non-uniform sampling (NUS) to obtain high-resolution spectra in less than 10 min. The combined strategy overcomes the signal overlap limitation in 1H NMR and the long acquisition time in traditional HSQC. The present results showed that twelve well-separated resonance peaks can be assigned in the bs-HSQC spectra, which are of high resolution, good repeatability, and precision. Notably, the identification accuracy of species was found to be 100% for all tests conducted in the present study. Furthermore, in combination with multivariate statistical methods, the proposed method can effectively determine the composition proportion of adulterants (from 10% to 90%). Based on the PLS-DA models, the identification accuracy was greater than 80% when composition proportion of adulterants was 10%. Thus, the proposed method may provide a fast, practical, and effective analysis technique for food quality control or authenticity identification. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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12 pages, 1893 KiB  
Article
Isolation and Characterization of an Unknown Process-Related Impurity in Furosemide and Validation of a New HPLC Method
by Ao Xu, Yunlin Xue, Yuyu Zeng, Jing Li, Huiling Zhou, Zhen Wang, Yin Chen, Hui Chen, Jian Jin and Tao Zhuang
Molecules 2023, 28(5), 2415; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28052415 - 06 Mar 2023
Viewed by 1978
Abstract
Furosemide is a widely used loop diuretic in the treatment of congestive heart failure and edema. During the preparation of furosemide, a new process-related impurity G in the levels ranging from 0.08% to 0.13% was detected in pilot batches by a new high [...] Read more.
Furosemide is a widely used loop diuretic in the treatment of congestive heart failure and edema. During the preparation of furosemide, a new process-related impurity G in the levels ranging from 0.08% to 0.13% was detected in pilot batches by a new high performance liquid chromatography (HPLC) method. The new impurity was isolated and characterized by comprehensive analysis of FT-IR, Q-TOF/LC-MS, 1D-NMR (1H, 13C, and DEPT), and 2D-NMR (1H-1H-COSY, HSQC, and HMBC) spectroscopy data. The possible formation pathway of impurity G was also discussed in detail. Moreover, a novel HPLC method was developed and validated for the determination of impurity G and the other six known impurities registered in the European Pharmacopoeia as per ICH guidelines. The HPLC method was validated with respect to system suitability, linearity, the limit of quantitation, the limit of detection, precision, accuracy, and robustness. The characterization of impurity G and the validation of its quantitative HPLC method were reported for the first time in this paper. Finally, the toxicological properties of impurity G were predicted by the in silico webserver ProTox-II. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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13 pages, 2006 KiB  
Article
Study on Molecularly Imprinted Polymers Obtained Sonochemically for the Determination of Aflatoxins in Food
by Sara Palmieri, Dounia Elfadil, Federico Fanti, Flavio Della Pelle, Manuel Sergi, Aziz Amine and Dario Compagnone
Molecules 2023, 28(2), 703; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28020703 - 10 Jan 2023
Cited by 6 | Viewed by 1549
Abstract
Aflatoxins (AFs) are fungi secondary metabolites produced by the Aspergillus family. These compounds can enter the food chain through food contamination, representing a risk to human health. Commercial immunoaffinity columns are widely used for the extraction and cleanup of AFs from food samples; [...] Read more.
Aflatoxins (AFs) are fungi secondary metabolites produced by the Aspergillus family. These compounds can enter the food chain through food contamination, representing a risk to human health. Commercial immunoaffinity columns are widely used for the extraction and cleanup of AFs from food samples; however, their high cost and large solvent consumption create a need for alternative strategies. In this work, an alternative strategy for producing molecularly imprinted polymers (MIPs) was proposed to extract aflatoxins AFB1, AFB2, AFG1, and AFG2 from complex food samples, using liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS). The MIPs were synthesized via a low-cost and rapid (5 min) sonochemical free-radical polymerization, using 1-hydroxy-2-naphthoic acid as a dummy template. MIPs-based solid phase extraction performance was tested on 17 dietary supplements (vegetables, fruits, and cereals), obtaining appreciable recovery rates (65–90%) and good reproducibility (RSD ≤ 6%, n = 3); the selectivity towards other mycotoxins was proved and the data obtained compared with commercial immunoaffinity columns. The proposed strategy can be considered an alternative affordable approach to the classical immunoaffinity columns, since it is more selective and better performing. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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12 pages, 1347 KiB  
Article
Rapid Analysis of Aristolochic Acids and Aristolactams in Houttuyniae Herba by LC–MS/MS
by Yingxue Wu, Jing Liu, Shuai Kang, Zhong Dai and Shuangcheng Ma
Molecules 2022, 27(24), 8969; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27248969 - 16 Dec 2022
Cited by 3 | Viewed by 1283
Abstract
Houttuyniae herba, the Saururaceae plant Houttuynia cordata Thunb., has multiple therapeutic effects, including clearing heat, eliminating toxins, reducing swelling, discharging pus, and relieving stagnation. It has a long history as an edible and medicinal plant in China. Phytochemical studies show that the main [...] Read more.
Houttuyniae herba, the Saururaceae plant Houttuynia cordata Thunb., has multiple therapeutic effects, including clearing heat, eliminating toxins, reducing swelling, discharging pus, and relieving stagnation. It has a long history as an edible and medicinal plant in China. Phytochemical studies show that the main constituents include volatile oil, flavonoids, and alkaloids. Aristolactam is a major alkaloid with a structure similar to toxic aristolochic acids. However, there has been no systematic study on aristolochic acids and alkaloids in Houttuyniae herba. Therefore, in this study, an LC–MS/MS method was developed to simultaneously detect seven alkaloids and five aristolochic acids in Houttuyniae herba from different origins. Six alkaloids (O-demethyl nornucifrine, N-nornucifrine, aristololactam AII, aristololactam FI, aristololactam BII, cepharadione B) were found and quantitatively determined in 75 batches of samples. Meanwhile, no aristolochic acids or aristololactams were found in Houttuyniae herba at a limit of detection (LOD) of ≤4 ng/mL. The method developed was fully validated in terms of LOD, limit of quantification (LOQ), linearity, precision, accuracy, and stability. These data clarify the content of the above safety-related components in Houttuyniae herba and provide a reference for further research into its safety. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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16 pages, 2451 KiB  
Article
Development and Validation of a UPLC-MS/MS Method for the Quantification of Components in the Ancient Classical Chinese Medicine Formula of Guyinjian
by Nan Ge, Zhineng Li, Le Yang, Guangli Yan, Aihua Zhang, Xiwu Zhang, Xiuhong Wu, Hui Sun, Dan Li and Xijun Wang
Molecules 2022, 27(23), 8611; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27238611 - 06 Dec 2022
Cited by 1 | Viewed by 1336
Abstract
Guyinjian (GYJ) is an ancient classic formula of traditional Chinese medicine used for the treatment of liver and kidney yin deficiency; it was derived from the book “Jing Yue Quan Shu” in the Ming Dynasty. Modern clinical observation experiments have shown that GYJ [...] Read more.
Guyinjian (GYJ) is an ancient classic formula of traditional Chinese medicine used for the treatment of liver and kidney yin deficiency; it was derived from the book “Jing Yue Quan Shu” in the Ming Dynasty. Modern clinical observation experiments have shown that GYJ has a definite therapeutic effect on the treatment of gynecological diseases such as kidney deficiency type oligomenorrhea, climacteric syndrome, intermenstrual bleeding, pubertal metrorrhagia, etc. However, the lack of GYJ quality control studies has greatly limited the development of its wider clinical application. In this study, a validated UPLC-MS/MS method was developed successfully for the first time and used to quantify fourteen compounds in GYJ samples with good specificity, linearity (r = 0.9960−0.9999), precision (RSD% ≤ 3.18%), stability (RSD% ≤ 2.22%) and accuracy (recovery test within 88.64–107.43%, RSD% at 2.82–6.22%). Simultaneously, the determination results of 15 batches of GYJ samples were analyzed by multivariate statistical methods, and it was found that the compounds have a greater influence on batch-to-batch stability, mainly Rehmannioside D, Loganin, Morroniside, Ginsenoside Re, and 3′,6-Disinapoylsucrose. The proposed new method has the advantages of high sensitivity, high selectivity, and rapid analysis, which provides a reference for the GYJ quality control study. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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17 pages, 2439 KiB  
Article
Chemical Profiling and Quantification of Potential Bioactive Components in Gandouling Pill by Ultra-High Performance Liquid Chromatography Coupled with Diode Array Detector/Quadruple-Qrbitrap Mass Spectrometry
by Yue Yang, Wenjie Hao, Yulong Yang, Shijie Zhang, Han Wang, Meixia Wang, Ting Dong, Zhanpeng Shang and Wenming Yang
Molecules 2022, 27(23), 8247; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27238247 - 26 Nov 2022
Viewed by 2043
Abstract
Gandouling (GDL) Pill is a novel Traditional Chinese medicinal drug to treat Wilson’s disease in clinics. It is composed of six separate herbal medicines, including Rhei Radix ET Rhizoma, Coptidis Rhizoma, Salviae Miltiorrhizae Radix ET Rhizoma, Spatholobi Caulis, Curcumae Rhizoma, and Curcumae Longae [...] Read more.
Gandouling (GDL) Pill is a novel Traditional Chinese medicinal drug to treat Wilson’s disease in clinics. It is composed of six separate herbal medicines, including Rhei Radix ET Rhizoma, Coptidis Rhizoma, Salviae Miltiorrhizae Radix ET Rhizoma, Spatholobi Caulis, Curcumae Rhizoma, and Curcumae Longae Rhizoma. In this study, a strategy was proposed to investigate the chemical constituents and to quantify the potential bioactive components in GDL Pill. Firstly, the mass fragmentation behaviors of representative compounds were investigated, and, in total, 69 compounds were characterized in GDL Pill using full scan/dd-MS2 scan mode by ultra-high-performance liquid chromatography (UPLC)/Q-Orbitrap mass spectrometry (MS). These compounds included 18 alkaloids, 18 ketones, 16 phenolic compounds, 11 organic acids, and 6 tanshinones. Seventeen of the compounds were unambiguously identified by comparison with reference standards. Secondly, the absorption components of GDL Pill in rat plasma were investigated by using target-Selected Ion Monitoring (t-SIM) scan mode built in Q-Orbitrap MS. A total of 18 components were detected, which were considered as potential bioactive components of GDL Pill. Thirdly, 10 major absorption components were simultaneously determined in six batches of samples by UPLC/diode array detector (DAD). The method was fully validated with respect to linearity, precision, repeatability, stability, and recovery. Alkaloids from Coptidis Rhizoma, such as coptisine (8), berberine (18), palmatine (19), were the most abundant bioactive compounds for GDL Pill that possess the potential be used as quality markers. The proposed strategy is practical and efficient for revealing the material basis of GDL Pill, and also provides a simple and accurate method for quality control. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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13 pages, 3219 KiB  
Article
Application of Deep-Learning Algorithm Driven Intelligent Raman Spectroscopy Methodology to Quality Control in the Manufacturing Process of Guanxinning Tablets
by Yi Tao, Jiaqi Bao, Qing Liu, Li Liu and Jieqiang Zhu
Molecules 2022, 27(20), 6969; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27206969 - 17 Oct 2022
Cited by 3 | Viewed by 1385
Abstract
Coupled with the convolutional neural network (CNN), an intelligent Raman spectroscopy methodology for rapid quantitative analysis of four pharmacodynamic substances and soluble solid in the manufacture process of Guanxinning tablets was established. Raman spectra of 330 real samples were collected by a portable [...] Read more.
Coupled with the convolutional neural network (CNN), an intelligent Raman spectroscopy methodology for rapid quantitative analysis of four pharmacodynamic substances and soluble solid in the manufacture process of Guanxinning tablets was established. Raman spectra of 330 real samples were collected by a portable Raman spectrometer. The contents of danshensu, ferulic acid, rosmarinic acid, and salvianolic acid B were determined with high-performance liquid chromatography-diode array detection (HPLC-DAD), while the content of soluble solid was determined by using an oven-drying method. In the establishing of the CNN calibration model, the spectral characteristic bands were screened out by a competitive adaptive reweighted sampling (CARS) algorithm. The performance of the CNN model is evaluated by root mean square error of calibration (RMSEC), root mean square error of cross-validation (RMSECV), root mean square error of prediction (RMSEP), coefficient of determination of calibration (Rc2), coefficient of determination of cross-validation (Rcv2), and coefficient of determination of validation (Rp2). The Rp2 values for soluble solid, salvianolic acid B, danshensu, ferulic acid, and rosmarinic acid are 0.9415, 0.9246, 0.8458, 0.8667, and 0.8491, respectively. The established model was used for the analysis of three batches of unknown samples from the manufacturing process of Guanxinning tablets. As the results show, Raman spectroscopy is faster and more convenient than that of conventional methods, which is helpful for the implementation of process analysis technology (PAT) in the manufacturing process of Guanxinning tablets. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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13 pages, 1651 KiB  
Article
Qualitative Analysis of Multiple Phytochemical Compounds in Tojapride Based on UHPLC Q-Exactive Orbitrap Mass Spectrometry
by Liying Zhang, Shihan Qin, Sunv Tang, Shuai E, Kailin Li, Jing Li, Wei Cai, Lei Sun and Hui Li
Molecules 2022, 27(19), 6639; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27196639 - 06 Oct 2022
Cited by 1 | Viewed by 1450
Abstract
Tojapride is composed of Caulis Perillae, Rhizoma Cyperi, Radix Glycyrrhizae, Citrus aurantium L., Coptis chinensis Franch, Pericarpium Citri Reticulatae, Reynoutria japonica Houtt, Tetradium ruticarpum, and Cleistocactus sepium. It has the effects of inhibiting gastric acid and relieving pain. It is clinically [...] Read more.
Tojapride is composed of Caulis Perillae, Rhizoma Cyperi, Radix Glycyrrhizae, Citrus aurantium L., Coptis chinensis Franch, Pericarpium Citri Reticulatae, Reynoutria japonica Houtt, Tetradium ruticarpum, and Cleistocactus sepium. It has the effects of inhibiting gastric acid and relieving pain. It is clinically used for treating gastroesophageal reflux disease. To further study the pharmacodynamic properties of Tojapride, the systematic characterization of the chemical constituents in Tojapride was investigated using ultra-performance liquid chromatography with Q-Exactive Orbitrap mass spectrometry combined with parallel reaction monitoring for the first time. Eventually, a total of 222 compounds, including flavonoids, alkaloids, and glycyrrhizic acid derivatives, were identified based on the chromatographic retention times, MS/MS2 information, and bibliography data; a total of 218 of these were reported for the first time as being present in Tojapride. This newly developed approach provides a powerful tool for extending our understanding of chemical constituents of Tojapride, which can be further extended to other TCMP composition research. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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12 pages, 2756 KiB  
Article
Detection and Quantification of Alprazolam Added to Long Drinks by Near Infrared Spectroscopy and Chemometrics
by Claudia Scappaticci, Stella Spera, Alessandra Biancolillo and Federico Marini
Molecules 2022, 27(19), 6420; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27196420 - 28 Sep 2022
Cited by 3 | Viewed by 1940
Abstract
In the present work, a fast, relatively cheap, and green analytical strategy to identify and quantify the fraudulent (or voluntary) addition of a drug (alprazolam, the API of Xanax®) to an alcoholic drink of large consumption, namely gin and tonic, was [...] Read more.
In the present work, a fast, relatively cheap, and green analytical strategy to identify and quantify the fraudulent (or voluntary) addition of a drug (alprazolam, the API of Xanax®) to an alcoholic drink of large consumption, namely gin and tonic, was developed using coupling near-infrared spectroscopy (NIR) and chemometrics. The approach used was both qualitative and quantitative as models were built that would allow for highlighting the presence of alprazolam with high accuracy, and to quantify its concentration with, in many cases, an acceptable error. Classification models built using partial least squares discriminant analysis (PLS-DA) allowed for identifying whether a drink was spiked or not with the drug, with a prediction accuracy in the validation phase often higher than 90%. On the other hand, calibration models established through the use of partial least squares (PLS) regression allowed for quantifying the drug added with errors of the order of 2–5 mg/L. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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17 pages, 2998 KiB  
Article
Multiple Fingerprints and Spectrum-Effect Relationship of Polysaccharides from Saposhnikoviae Radix
by Mengqi Yu, Guang Xu, Ming Qin, Yanling Li, Yuying Guo and Qun Ma
Molecules 2022, 27(16), 5278; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27165278 - 18 Aug 2022
Cited by 11 | Viewed by 1631
Abstract
PMP-HPLC, FT-IR, and HPSEC fingerprints of 10 batches of polysaccharides from Saposhnikoviae Radix with different production areas and harvest times have been prepared, and the chemometrics analysis was performed. The anti-allergic activity of 10 batches of Saposhnikoviae Radix polysaccharide (SP) was evaluated, and [...] Read more.
PMP-HPLC, FT-IR, and HPSEC fingerprints of 10 batches of polysaccharides from Saposhnikoviae Radix with different production areas and harvest times have been prepared, and the chemometrics analysis was performed. The anti-allergic activity of 10 batches of Saposhnikoviae Radix polysaccharide (SP) was evaluated, and the spectrum-effect relationship of the 10 batches of SP was analyzed by gray correlation degree with the chromatographic fingerprint as the independent variable. The results showed that the PMP-HPLC, HPSEC, and FT-IR fingerprints of 10 batches of SP had a high similarity. Two monosaccharides (rhamnose and galactose), the polysaccharide fragment Mn = 8.67 × 106~9.56 × 106 Da, and the FT-IR absorption peak of 892 cm−1 can be used as the quality control markers of SPs. All 10 batches of SP could significantly inhibit the release of β-HEX in RBL-231 cells, and the polysaccharides harvested from Inner Mongolia in the winter had the best anti-allergic activity. The spectrum-effect relationship model showed that the monosaccharide composition and molecular weight were related to the anti-allergic activity of the SPs. Multiple fingerprints combined with spectrum-effect relationship analysis can evaluate and control the quality of SPs from the aspects of overall quality and efficacy, which has more application value. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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11 pages, 1305 KiB  
Article
Simultaneous Determination of 21 Sulfonamides in Poultry Eggs Using Ionic Liquid-Modified Molecularly Imprinted Polymer SPE and UPLC–MS/MS
by Decheng Suo, Su Zhang, Zhanteng Song, Shi Wang, Yang Li and Xia Fan
Molecules 2022, 27(15), 4953; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27154953 - 04 Aug 2022
Cited by 3 | Viewed by 1451
Abstract
An ionic liquid-modified molecularly imprinted polymer (IL-MIP) composite with sulfamethazine as a template molecule and methyl acrylic acid and 1-aminopropyl-3-methylimidazolium bromide as functional monomers was successfully synthesized. The achieved IL-MIP was characterized and evaluated in detail and utilized in the extraction and cleanup [...] Read more.
An ionic liquid-modified molecularly imprinted polymer (IL-MIP) composite with sulfamethazine as a template molecule and methyl acrylic acid and 1-aminopropyl-3-methylimidazolium bromide as functional monomers was successfully synthesized. The achieved IL-MIP was characterized and evaluated in detail and utilized in the extraction and cleanup of sulfonamides (SAs) in poultry egg samples. The results demonstrated that the IL-MIP possessed a broad reorganization toward SAs and could selectively adsorb 21 kinds of SA compounds. Furthermore, the solid-phase extraction column based on the IL-MIP was used in the extraction and cleanup of 21 SAs in eggs, and the confirmatory detection of SAs was performed using ultraperformance liquid chromatography–tandem mass spectrometry. Under optimum conditions, the limits of detection (LODs) for all SAs ranged from 0.1 ng·g−1 to 1.5 ng·g−1, and the LOD of this method was better than those of the existing methods. The recoveries of SA compounds spiked in egg samples ranged from 84.3% to 105.8%, with low relative standard deviations (<15%). The developed method based on the IL-MIP extraction and cleanup was successfully used in the detection of 21 SAs in more than 100 real poultry egg samples. The results indicated that the proposed method was suitable for detecting 21 SAs in poultry eggs. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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15 pages, 3731 KiB  
Article
Effect of Different Processing Methods on the Chemical Constituents of Scrophulariae Radix as Revealed by 2D NMR-Based Metabolomics
by Xiaohui Duan, Mina Zhang, Huan Du, Xiu Gu, Caihong Bai, Liuqiang Zhang, Kaixian Chen, Kaifeng Hu and Yiming Li
Molecules 2022, 27(15), 4687; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27154687 - 22 Jul 2022
Cited by 3 | Viewed by 1594
Abstract
Scrophulariae Radix (SR) is one of the oldest and most frequently used Chinese herbs for oriental medicine in China. Before clinical use, the SR should be processed using different methods after harvest, such as steaming, “sweating”, and traditional fire-drying. In order to investigate [...] Read more.
Scrophulariae Radix (SR) is one of the oldest and most frequently used Chinese herbs for oriental medicine in China. Before clinical use, the SR should be processed using different methods after harvest, such as steaming, “sweating”, and traditional fire-drying. In order to investigate the difference in chemical constituents using different processing methods, the two-dimensional (2D) 1H-13C heteronuclear single quantum correlation (1H-13C HSQC)-based metabolomics approach was applied to extensively characterize the difference in the chemical components in the extracts of SR processed using different processing methods. In total, 20 compounds were identified as potential chemical markers that changed significantly with different steaming durations. Seven compounds can be used as potential chemical markers to differentiate processing by sweating, hot-air drying, and steaming for 4 h. These findings could elucidate the change of chemical constituents of the processed SR and provide a guide for the processing. In addition, our protocol may represent a general approach to characterizing chemical compounds of traditional Chinese medicine (TCM) and therefore might be considered as a promising approach to exploring the scientific basis of traditional processing of TCM. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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11 pages, 1883 KiB  
Article
Surface Functionalized Magnetic Nanoparticles as a Selective Sorbent for Affinity Fishing of PPAR-γ Ligands from Choerospondias axillaris
by Miaomiao Chi, Kunming Qin, Lei Cao, Min Zhang, Yingying Su and Xun Gao
Molecules 2022, 27(10), 3127; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27103127 - 13 May 2022
Cited by 2 | Viewed by 1556
Abstract
Coronary heart disease (CHD), which has developed into one of the major diseases, was reported to be treated by the target of peroxisome proliferators-activate receptor γ (PPAR-γ). As a natural medicine long used in the treatment of CHD, there are few studies on [...] Read more.
Coronary heart disease (CHD), which has developed into one of the major diseases, was reported to be treated by the target of peroxisome proliferators-activate receptor γ (PPAR-γ). As a natural medicine long used in the treatment of CHD, there are few studies on how to screen the target active compounds with high specific activity from Choerospondias axillaris. To advance the pace of research on target-specific active compounds in natural medicines, we have combined magnetic ligand fishing and functionalized nano-microspheres to investigate the active ingredients of PPAR-γ targets in Choerospondias axillaris. The PPAR-γ functionalized magnetic nano-microspheres have been successfully synthesized and characterized by vibrating sample magnetometer (VSM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The specificity, reusability, and reproducibility of the nano-microspheres were investigated with the help of the specific binding of rosiglitazone to PPAR-γ. In addition, the incubation temperature and the pH of the buffer solution in the magnetic ligand fishing were optimized to improve the specific adsorption efficiency of the analytes. Finally, with the aid of ultraperformance liquid chromatography plus Q-Exactive Orbitrap tandem mass spectrometry (UHPLC-Q-Exactive Orbitrap-MS/MS), the 16 active ligands including 9 organic acids, 5 flavonoids, and 2 phenols were found in the ethanolic extracts of Choerospondias axillaris. Therefore, the study can provide a successful precedent for realizing the designated extraction and rapid isolation of target-specific active ingredient groups in the complex mixtures. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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Review

Jump to: Research

20 pages, 989 KiB  
Review
Comprehensive Extraction and Chemical Characterization of Bioactive Compounds in Tepals of Crocus sativus L.
by Fabrizio Ruggieri, Maria Anna Maggi, Michela Rossi and Roberto Consonni
Molecules 2023, 28(16), 5976; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28165976 - 09 Aug 2023
Cited by 1 | Viewed by 1127
Abstract
Crocus sativus L. is largely cultivated because it is the source of saffron, a well-appreciated and valued spice, not only for its culinary use but also because of its significant biological activities. Stigmas are the main product obtained from flowers, but in addition, [...] Read more.
Crocus sativus L. is largely cultivated because it is the source of saffron, a well-appreciated and valued spice, not only for its culinary use but also because of its significant biological activities. Stigmas are the main product obtained from flowers, but in addition, tepals, largely considered a waste product, represent a big source of flavonoids and anthocyanins. This study aimed to delve into the phytochemical composition of saffron tepals and investigate whether the composition was influenced by the extraction technique while investigating the main analytical techniques most suitable for the characterization of tepal extracts. The research focuses on flavonoids, a class of secondary metabolites, and their health benefits, including antioxidant, anti-inflammatory, and anticancer properties. Flavonoids occur as aglycones and glycosides and are classified into various classes, such as flavones, flavonols, and flavanones. The most abundant flavonoids in tepals are kaempferol glycosides, followed by quercetin and isorhamnetin glycosides. Overall, this review provides valuable insights into the potential uses of tepals as a source of bioactive compounds and their applications in various fields, promoting a circular and sustainable economy in saffron cultivation and processing. Full article
(This article belongs to the Special Issue Advanced Analytical Tools for Characterization and Quality Control of Food, Drugs, and Natural Active Ingredients)
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