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Advances in Chemical Analysis Procedures (Part I): Extraction and Instrument Configuration

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

Deadline for manuscript submissions: closed (31 December 2019) | Viewed by 46876

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Special Issue Editors

Dr. Marcello Locatelli

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Department of Pharmacy, University “G. d\'Annunzio” of Chieti and Pescara, Chieti, Italy
Interests: innovative (micro)extraction procedures; hyphenated instrument configurations; bioactive compounds; characterization; fingerprints; method validation; HPLC; mass spectrometry; biological matrices; chromatography; analytical chemistry; sample preparation; green analytical methodologies
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Dr. Angela Tartaglia

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Department of Pharmacy, University "G. d'Annunzio" of Chieti-Pescara, Build B, level II, Via dei Vestini, 31, 66100 Chieti (CH), Italy
Interests: method development; analytical and bioanalytical chemistry; method validation; hyphenated assay; HPLC
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Prof. Dr. Dora Melucci

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Department of Chemistry “Giacomo Ciamician”, Alma Mater Studiorum University of Bologna, Via Selmi 2, I-40126 Bologna, Italy
Interests: chemometrics; environmental chemistry; forensics; food chemistry; pharmaceutics
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Prof. Dr. Abuzar Kabir

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International Forensic Research Institute, Department of Chemistry and Biochemistry, Florida International University, Miami, FL, USA
Interests: chromatographic stationary phases; substrate-free solid-phase extraction sorbents; molecular imprinting technology; sorbents for environmental pollution remediation; miniaturized sample preparation devices; field deployable sample preparation technology
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Prof. Dr. Halil Ibrahim Ulusoy

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Department of Analytical Chemistry, Faculty of Pharmacy, Cumhuriyet University, 58140 Sivas, Turkey
Interests: analytical method development; chromatography; pre-concentration and seperation methods; trace analysis; molecular and atomic spectroscopy
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Prof. Dr. Victoria Samanidou

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Laboratory of Analytical Chemistry, School of Chemistry, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece
Interests: analytical chemistry; sample preparation; chromatography; HPLC; method validation; method development; separation science; food analysis; bioanalysis; environmental analysis; green analytical chemistry; sorptive extraction; microextraction techniques
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Innovative analytical protocols are needed during all processes involved in chemical analysis, to establish the identities, properties, pureness, bioactivities, quantities, and other main features. Furthermore, modern analytical methods provide accurate information about therapeutic dosage and/or pharmacokinetics about new chemical entities (NCE). During the last few years, new techniques for chemical analysis have been developed which allow separation scientists to get all relevant information quickly and accurately even when the analysis is carried out in complex matrices (biological fluids, environmental samples, or food matrices). This Special Issue will highlight and describe the latest innovations in instruments and techniques developed for the extraction, analysis, and characterization of drugs, bioactive compounds, and pollutants in samples that until recently were difficult to analyze. Greater attention will be paid to recent developments in sample preparation and extraction techniques, with a focus on modern detection techniques, starting with one of the stalwarts of analytical chemistry laboratories, high-performance liquid chromatography (HPLC), up to more innovative instrumentation such as mass spectrometry, mostly used in biological sciences for detection and quantization of protein.

Subtopics: Analytical instrumental procedures; extraction procedures; novel technologies for analytical chemistry; isolation and clean-up procedures.

Schedule: Manuscript submission deadline: July 2019
Peer Review Due: August 2019
Revision Due: September 2019
Notification of acceptance by the Guest Editors: September 2019
Final manuscripts due: October 2019

Prof. Dr. Marcello Locatelli
Dr. Angela Tartaglia
Dr. Dora Melucci
Dr. Abuzar Kabir
Prof. Dr. Halil Ibrahim Ulusoy
Prof. Dr. Victoria Samanidou
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

Innovative techniques
Extraction procedures
Instrument configurations
Complex matrices

Published Papers (9 papers)

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Research

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18 pages, 1352 KiB

Open AccessArticle

Screening 89 Pesticides in Fishery Drugs by Ultrahigh Performance Liquid Chromatography Tandem Quadrupole-Orbitrap Mass Spectrometer

by Shou-Ying Wang, Cong Kong, Qing-Ping Chen and Hui-Juan Yu

Molecules 2019, 24(18), 3375; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules24183375 - 17 Sep 2019

Cited by 5 | Viewed by 2975

Abstract

Multiclass screening of drugs with high resolution mass spectrometry is of great interest due to its high time-efficiency and excellent accuracy. A high-scale, fast screening method for pesticides in fishery drugs was established based on ultrahigh performance liquid chromatography tandem quadrupole-Orbitrap high-resolution mass spectrometer. The target compounds - were diluted in methanol and extracted by ultrasonic treatment, and the extracts were diluted with MeOH-water (1:1, v/v) and centrifuged to remove impurities. The chromatographic separation was performed on an Accucore aQ-MS column (100 mm × 2.1 mm, 2.6 μm) with gradient elution using 0.1% formic acid in water (containing 5 mmol/L ammonium formate) and 0.1% formic acid in methanol (containing 5 mmol/L ammonium formate) in Full Scan/dd-MS2 (TopN) scan mode. A screening database, including mass spectrometric and chromatographic information, was established for identification of compounds. The screening detection limits of methods ranged between 1–500 mg/kg, the recoveries of real samples spiked with the concentration of 10 mg/kg and 100 mg/kg standard mixture ranged from 70% to 110% for more than sixty compounds, and the relative standard deviations (RSDs) were less than 20%. The application of this method showed that target pesticides were screened out in 10 samples out of 21 practical samples, in which the banned pesticide chlorpyrifos were detected in 3 out of the 10 samples. Full article

(This article belongs to the Special Issue Advances in Chemical Analysis Procedures (Part I): Extraction and Instrument Configuration)

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10 pages, 2120 KiB

Open AccessCommunication

Effects of Harvest Time on Phytochemical Constituents and Biological Activities of Panax ginseng Berry Extracts

by Seung-Yeap Song, Dae-Hun Park, Seong-Wook Seo, Kyung-Mok Park, Chun-Sik Bae, Hong-Seok Son, Hyung-Gyun Kim, Jung-Hee Lee, Goo Yoon, Jung-Hyun Shim, Eunok Im, Sang Hoon Rhee, In-Soo Yoon and Seung-Sik Cho

Molecules 2019, 24(18), 3343; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules24183343 - 13 Sep 2019

Cited by 5 | Viewed by 2882

Abstract

Ginseng (Panax ginseng) has long been used as a traditional medicine for the prevention and treatment of various diseases. Generally, the harvest time and age of ginseng have been regarded as important factors determining the efficacy of ginseng. However, most studies have mainly focused on the root of ginseng, while studies on other parts of ginseng such as its berry have been relatively limited. Thus, the aim of this study iss to determine effects of harvest time on yields, phenolics/ginsenosides contents, and the antioxidant/anti-elastase activities of ethanol extracts of three- and four-year-old ginseng berry. In both three- and fourfour-year-old ginseng berry extracts, antioxidant and anti-elastase activities tended to increase as berries ripen from the first week to the last week of July. Liquid chromatography-tandem mass spectrometry analysis has revealed that contents of ginsenosides except Rg1 tend to be the highest in fourfour-year-old ginseng berries harvested in early July. These results indicate that biological activities and ginsenoside profiles of ginseng berry extracts depend on their age and harvest time in July, suggesting the importance of harvest time in the development of functional foods and medicinal products containing ginseng berry extracts. To the best of our knowledge, this is the first report on the influence of harvest time on the biological activity and ginsenoside contents of ginseng berry extracts. Full article

(This article belongs to the Special Issue Advances in Chemical Analysis Procedures (Part I): Extraction and Instrument Configuration)

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10 pages, 1357 KiB

Open AccessArticle

Determination of Flavonoid Glycosides by UPLC-MS to Authenticate Commercial Lemonade

by Ying Xue, Lin-Sen Qing, Li Yong, Xian-Shun Xu, Bin Hu, Ming-Qing Tang and Jing Xie

Molecules 2019, 24(16), 3016; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules24163016 - 20 Aug 2019

Cited by 10 | Viewed by 3380

Abstract

So far, there is no report on the quality evaluation of lemonade available in the market. In this study, a sample preparation method was developed for the determination of flavonoid glycosides by ultra-performance liquid chromatography–mass spectrometry (UPLC-MS) based on vortex-assisted dispersive liquid-liquid microextraction. First, potential flavonoids in lemonade were scanned and identified by ultra-performance liquid chromatography–time of flight mass spectrometry (UPLC-TOF/MS). Five flavonoid glycosides were identified as eriocitrin, narirutin, hesperidin, rutin, and diosmin according to the molecular formula provided by TOF/MS and subsequent confirmation of the authentic standard. Then, an ultra-performance liquid chromatography–triple quadrupole mass spectrometry (UPLC-QqQ/MS) method was developed to determine these five flavonoid glycosides in lemonade. The results showed that the content of rutin in some lemonade was unreasonably high. We suspected that many illegal manufacturers achieved the goal of low-cost counterfeiting lemonade by adding rutin. This suggested that it was necessary for relevant departments of the state to make stricter regulations on the quality standards of lemonade beverages. Full article

(This article belongs to the Special Issue Advances in Chemical Analysis Procedures (Part I): Extraction and Instrument Configuration)

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23 pages, 5795 KiB

Open AccessArticle

Assessing Geographical Origin of Gentiana Rigescens Using Untargeted Chromatographic Fingerprint, Data Fusion and Chemometrics

by Tao Shen, Hong Yu and Yuan-Zhong Wang

Molecules 2019, 24(14), 2562; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules24142562 - 14 Jul 2019

Cited by 19 | Viewed by 3482

Abstract

Gentiana rigescens Franchet, which is famous for its bitter properties, is a traditional drug of chronic hepatitis and important raw materials for the pharmaceutical industry in China. In the study, high-performance liquid chromatography (HPLC), coupled with diode array detector (DAD) and chemometrics, were used to investigate the chemical geographical variation of G. rigescens and to classify medicinal materials, according to their grown latitudes. The chromatographic fingerprints of 280 individuals and 840 samples from rhizomes, stems, and leaves of four different latitude areas were recorded and analyzed for tracing the geographical origin of medicinal materials. At first, HPLC fingerprints of underground and aerial parts were generated while using reversed-phase liquid chromatography. After the preliminary data exploration, two supervised pattern recognition techniques, random forest (RF) and orthogonal partial least-squares discriminant analysis (OPLS-DA), were applied to the three HPLC fingerprint data sets of rhizomes, stems, and leaves, respectively. Furthermore, fingerprint data sets of aerial and underground parts were separately processed and joined while using two data fusion strategies (“low-level” and “mid-level”). The results showed that classification models that are based OPLS-DA were more efficient than RF models. The classification models using low-level data fusion method built showed considerably good recognition and prediction abilities (the accuracy is higher than 99% and sensibility, specificity, Matthews correlation coefficient, and efficiency range from 0.95 to 1.00). Low-level data fusion strategy combined with OPLS-DA could provide the best discrimination result. In summary, this study explored the latitude variation of phytochemical of G. rigescens and developed a reliable and accurate identification method for G. rigescens that were grown at different latitudes based on untargeted HPLC fingerprint, data fusion, and chemometrics. The study results are meaningful for authentication and the quality control of Chinese medicinal materials. Full article

(This article belongs to the Special Issue Advances in Chemical Analysis Procedures (Part I): Extraction and Instrument Configuration)

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12 pages, 845 KiB

Open AccessEditor’s ChoiceArticle

Fast Detection of 10 Cannabinoids by RP-HPLC-UV Method in Cannabis sativa L.

by Mara Mandrioli, Matilde Tura, Stefano Scotti and Tullia Gallina Toschi

Molecules 2019, 24(11), 2113; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules24112113 - 04 Jun 2019

Cited by 60 | Viewed by 11693

Abstract

Cannabis has regained much attention as a result of updated legislation authorizing many different uses and can be classified on the basis of the content of tetrahydrocannabinol (THC), a psychotropic substance for which there are legal limitations in many countries. For this purpose, accurate qualitative and quantitative determination is essential. The relationship between THC and cannabidiol (CBD) is also significant as the latter substance is endowed with many specific and non-psychoactive proprieties. For these reasons, it becomes increasingly important and urgent to utilize fast, easy, validated, and harmonized procedures for determination of cannabinoids. The procedure described herein allows rapid determination of 10 cannabinoids from the inflorescences of Cannabis sativa L. by extraction with organic solvents. Separation and subsequent detection are by RP-HPLC-UV. Quantification is performed by an external standard method through the construction of calibration curves using pure standard chromatographic reference compounds. The main cannabinoids dosed (g/100 g) in actual samples were cannabidiolic acid (CBDA), CBD, and Δ9-THC (Sample L11 CBDA 0.88 ± 0.04, CBD 0.48 ± 0.02, Δ9-THC 0.06 ± 0.00; Sample L5 CBDA 0.93 ± 0.06, CBD 0.45 ± 0.03, Δ9-THC 0.06 ± 0.00). The present validated RP-HPLC-UV method allows determination of the main cannabinoids in Cannabis sativa L. inflorescences and appropriate legal classification as hemp or drug-type. Full article

(This article belongs to the Special Issue Advances in Chemical Analysis Procedures (Part I): Extraction and Instrument Configuration)

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15 pages, 1989 KiB

Open AccessArticle

Synthesis of Graphene Oxide Based Sponges and Their Study as Sorbents for Sample Preparation of Cow Milk Prior to HPLC Determination of Sulfonamides

by Martha Maggira, Eleni A. Deliyanni and Victoria F. Samanidou

Molecules 2019, 24(11), 2086; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules24112086 - 31 May 2019

Cited by 19 | Viewed by 3675

Abstract

In the present study, a novel, simple, and fast sample preparation technique is described for the determination of four sulfonamides (SAs), namely Sulfathiazole (STZ), sulfamethizole (SMT), sulfadiazine (SDZ), and sulfanilamide (SN) in cow milk prior to HPLC. This method takes advantage of a novel material that combines the extractive properties of graphene oxide (GO) and the known properties of common polyurethane sponge (PU) and that makes sample preparation easy, fast, cheap and efficient. The PU-GO sponge was prepared by an easy and fast procedure and was characterized with FTIR spectroscopy. After the preparation of the sorbent material, a specific extraction protocol was optimized and combined with HPLC-UV determination could be applied for the sensitive analysis of trace SAs in milk. The proposed method showed good linearity while the coefficients of determination (R²) were found to be high (0.991–0.998). Accuracy observed was within the range 90.2–112.1% and precision was less than 12.5%. Limit of quantification for all analytes in milk was 50 μg kg⁻¹. Furthermore, the PU-GO sponge as sorbent material offered a very clean extract, since no matrix effect was observed. Full article

(This article belongs to the Special Issue Advances in Chemical Analysis Procedures (Part I): Extraction and Instrument Configuration)

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16 pages, 1052 KiB

Open AccessArticle

Liquid Phase and Microwave-Assisted Extractions for Multicomponent Phenolic Pattern Determination of Five Romanian Galium Species Coupled with Bioassays

by Andrei Mocan, Alina Diuzheva, Sabin Bădărău, Cadmiel Moldovan, Vasil Andruch, Simone Carradori, Cristina Campestre, Angela Tartaglia, Marta De Simone, Dan Vodnar, Matteo Tiecco, Raimondo Germani, Gianina Crișan and Marcello Locatelli

Molecules 2019, 24(7), 1226; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules24071226 - 28 Mar 2019

Cited by 24 | Viewed by 3867

Abstract

Background: Galium is a plant rich in iridoid glycosides, flavonoids, anthraquinones, and small amounts of essential oils and vitamin C. Recent works showed the antibacterial, antifungal, antiparasitic, and antioxidant activity of this plant genus. Methods: For the determination of the multicomponent phenolic pattern, liquid phase microextraction procedures were applied, combined with HPLC-PDA instrument configuration in five Galium species aerial parts (G. verum, G. album, G. rivale, G. pseudoaristatum, and G. purpureum). Dispersive Liquid–Liquid MicroExtraction (DLLME) with NaCl and NAtural Deep Eutectic Solvent (NADES) medium and Ultrasound-Assisted (UA)-DLLME with β-cyclodextrin medium were optimized. Results: The optimal DLLME conditions were found to be: 10 mg of the sample, 10% NaCl, 15% NADES or 1% β-cyclodextrin as extraction solvent—400 μL of ethyl acetate as dispersive solvent—300 μL of ethanol, vortex time—30 s, extraction time—1 min, centrifugation at 12000× g for 5 min. Conclusions: These results were compared with microwave-assisted extraction procedures. G. purpureum and G. verum extracts showed the highest total phenolic and flavonoid content, respectively. The most potent extract in terms of antioxidant capacity was obtained from G. purpureum, whereas the extract obtained from G. album exhibited the strongest inhibitory effect against tyrosinase. Full article

(This article belongs to the Special Issue Advances in Chemical Analysis Procedures (Part I): Extraction and Instrument Configuration)

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Review

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20 pages, 789 KiB

Open AccessReview

An Update on Isolation Methods for Proteomic Studies of Extracellular Vesicles in Biofluids

by Jing Li, Xianqing He, Yuanyuan Deng and Chenxi Yang

Molecules 2019, 24(19), 3516; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules24193516 - 27 Sep 2019

Cited by 59 | Viewed by 6135

Abstract

Extracellular vesicles (EVs) are lipid bilayer enclosed particles which present in almost all types of biofluids and contain specific proteins, lipids, and RNA. Increasing evidence has demonstrated the tremendous clinical potential of EVs as diagnostic and therapeutic tools, especially in biofluids, since they can be detected without invasive surgery. With the advanced mass spectrometry (MS), it is possible to decipher the protein content of EVs under different physiological and pathological conditions. Therefore, MS-based EV proteomic studies have grown rapidly in the past decade for biomarker discovery. This review focuses on the studies that isolate EVs from different biofluids and contain MS-based proteomic analysis. Literature published in the past decade (2009.1–2019.7) were selected and summarized with emphasis on isolation methods of EVs and MS analysis strategies, with the aim to give an overview of MS-based EV proteomic studies and provide a reference for future research. Full article

(This article belongs to the Special Issue Advances in Chemical Analysis Procedures (Part I): Extraction and Instrument Configuration)

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24 pages, 7631 KiB

Open AccessReview

Determination of Kanamycin by High Performance Liquid Chromatography

by Xingping Zhang, Jiujun Wang, Qinghua Wu, Li Li, Yun Wang and Hualin Yang

Molecules 2019, 24(10), 1902; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules24101902 - 17 May 2019

Cited by 67 | Viewed by 7695

Abstract

Kanamycin is an aminoglycoside antibiotic widely used in treating animal diseases caused by Gram-negative and Gram-positive infections. Kanamycin has a relatively narrow therapeutic index, and can accumulate in the human body through the food chain. The abuse of kanamycin can have serious side-effects. Therefore, it was necessary to develop a sensitive and selective analysis method to detect kanamycin residue in food to ensure public health. There are many analytical methods to determine kanamycin concentration, among which high performance liquid chromatography (HPLC) is a common and practical tool. This paper presents a review of the application of HPLC analysis of kanamycin in different sample matrices. The different detectors coupled with HPLC, including Ultraviolet (UV)/Fluorescence, Evaporative Light Scattering Detector (ELSD)/Pulsed Electrochemical Detection (PED), and Mass Spectrometry, are discussed. Meanwhile, the strengths and weaknesses of each method are compared. The pre-treatment methods of food samples, including protein precipitation, liquid-liquid extraction (LLE), and solid-phase extraction (SPE) are also summarized in this paper. Full article

(This article belongs to the Special Issue Advances in Chemical Analysis Procedures (Part I): Extraction and Instrument Configuration)

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