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Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis

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

Deadline for manuscript submissions: closed (31 July 2018) | Viewed by 101705

Printed Edition Available!
A printed edition of this Special Issue is available here.

Special Issue Editors

Dr. Marcello Locatelli

E-Mail Website
Guest Editor
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
Special Issues, Collections and Topics in MDPI journals
Dr. Simone Carradori

E-Mail Website
Guest Editor
Department of Pharmacy, University “G. d'Annunzio” of Chieti-Pescara, Chieti, Italy
Interests: chemical modification of natural compounds; medicinal chemistry; food chemistry; antioxidants; antimicrobials
Special Issues, Collections and Topics in MDPI journals
Dr. Andrei Mocan

E-Mail Website
Guest Editor
Department of Pharmaceutical Botany, “Iuliu Hațieganu” University of Medicine and Pharmacy, Cluj-Napoca, Romania
Interests: plant-derived secondary metabolites; antimicrobials; antioxidants; enzyme inhibition
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Techniques that can be employed to accelerate extractions, work up, and isolation/purification of the products/metabolites, may be of interest both in the fields of natural products (food, plants, plant-derived products) and in analytical chemistry (biological matrices, clinical trials, sample preparation). In the last few years, the development of innovative procedures has deeply impacted the work of chemists.

The present Special Issue, “Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis”, aims to collect and to disseminate some of the most significant and recent contributions in the interdisciplinary area of innovative extraction procedures from complex matrices followed by validated analytical methods using hyphenated instrument configurations to support the optimization of the whole process and the scale-up possibility.

The scope is broad and includes the use of alternative (green) and/or innovative extraction techniques, optimization of the corresponding parameters by means of experimental design, development of proper solvents (ionic liquids, deep eutectic solvents, cyclodextrins), extract fractioning on the basis of specific biological activities, knowledge of the target structures in order to pursue a targeted analysis, and evaluation of the stability of intermediates/final products.

Accepted paper (both reviews and research papers) could be in the field of: - extraction procedures - hyphenated techniques - food and food supplements analyses - biological analyses - chemometric approaches. Eventually all related to specific biological activities observed.

- Abstract submission     February 2018

- Paper submission     31 May 2018

- Revision (Reviewer)     end of June 2018

- Revised version     end of July 2018

- Final proof     first days of September 2018

Prof. Dr. Marcello Locatelli
Prof. Dr. Simone Carradori
Dr. Andrei Mocan
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

  • hyphenated techniques
  • innovative (micro)extraction procedures
  • biological activities
  • food and food supplements analyses
  • medicinal plants and fungi
  • biological analyses
  • chemometric approaches

Published Papers (21 papers)

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Editorial

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3 pages, 151 KiB  
Editorial
Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis
by Marcello Locatelli, Simone Carradori and Andrei Mocan
Molecules 2018, 23(9), 2391; https://doi.org/10.3390/molecules23092391 - 18 Sep 2018
Cited by 1 | Viewed by 2692
Abstract
n/a Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)

Research

Jump to: Editorial, Review

28 pages, 1843 KiB  
Article
Process Optimization for Improved Phenolic Compounds Recovery from Walnut (Juglans regia L.) Septum: Phytochemical Profile and Biological Activities
by Marius Emil Rusu, Ana-Maria Gheldiu, Andrei Mocan, Cadmiel Moldovan, Daniela-Saveta Popa, Ioan Tomuta and Laurian Vlase
Molecules 2018, 23(11), 2814; https://doi.org/10.3390/molecules23112814 - 30 Oct 2018
Cited by 53 | Viewed by 5605
Abstract
Plant by-products can be valuable sources of polyphenol bioactive compounds. Walnut (Juglans regia L.) is a very important tree nut rich in biologically active molecules, but its septum was scarcely researched. Experimental data indicated a hypoglycemic effect of septum extracts, with almost [...] Read more.
Plant by-products can be valuable sources of polyphenol bioactive compounds. Walnut (Juglans regia L.) is a very important tree nut rich in biologically active molecules, but its septum was scarcely researched. Experimental data indicated a hypoglycemic effect of septum extracts, with almost no details about its phytochemical composition. The main objectives of this study were: (1) to obtain walnut septum (WS) extracts with high content in bioactive compounds and antioxidant activity based on an original experimental design; (2) characterization of the phytochemical profile of the WS extracts using HPLC-MS/MS; (3) evaluation of the biological potential of the richest polyphenolic WS extract. The variables of the experimental design were: extraction method (maceration and Ultra-Turrax extraction), temperature, solvent (acetone and ethanol), and percentage of water in the solvent. The first quantifiable responses were: total phenolic content, total flavonoid content, condensed tannins, and ABTS antioxidant capacity. The phytochemical profile of lyophilized extracts obtained by Ultra-Turrax extraction (UTE), the most efficient method, was further determined by HPLC-MS/MS analysis of individual polyphenolic and phytosterols compounds. It is the first study to assay the detailed composition of WS in hydrophilic and lipophilic compounds. The biological potential of the richest polyphenolic WS extract was also evaluated by FRAP and DPPH antioxidant capacity and the inhibition of tyrosinase, an enzyme involved in the browning in fruits and vegetables, skin wrinkles and aging. Conclusion: The phytochemical profile of the analyzed extracts proves that WS can be a valuable source of biologically active compounds (polyphenols) for food and/or pharmaceutical industry and warrant the continuation of current research in further evaluating its bioactive potential. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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8 pages, 738 KiB  
Communication
Ultra-High-Performance Liquid Chromatography Tandem Mass Spectrometry Assay for Determination of Endogenous GHB and GHB-Glucuronide in Nails
by Francesco Paolo Busardò, Massimo Gottardi, Anastasio Tini, Claudia Mortali, Raffaele Giorgetti and Simona Pichini
Molecules 2018, 23(10), 2686; https://doi.org/10.3390/molecules23102686 - 18 Oct 2018
Cited by 18 | Viewed by 3241
Abstract
Background: The short chain fatty acid gamma-hydroxybutyric acid (GHB) is a precursor, and the metabolite of gamma-aminobutyric acid is commonly used as an illegal recreational drug of abuse. Methods: An ultra-high-performance liquid chromatography tandem mass spectrometry was developed and validated for [...] Read more.
Background: The short chain fatty acid gamma-hydroxybutyric acid (GHB) is a precursor, and the metabolite of gamma-aminobutyric acid is commonly used as an illegal recreational drug of abuse. Methods: An ultra-high-performance liquid chromatography tandem mass spectrometry was developed and validated for endogenous GHB and its glucuronide in nails, to complement hair in forensic contexts for a retrospective detection of psychotropic drugs consumption. Results: GHB endogenous values for children and adolescents, adult females, and adult males in fingernails ranged from 0.3 to 3.0, 3.2, and 3.8 ng/mg, respectively, and toenails values ranged from 0.3 to 1.8, 2.0, and 2.4 ng/mg, respectively. In the three different groups, values of GHB in fingernails were statistically higher than those in toenails. GHB glucuronide could only be detected in finger nails with values ranging from 0.08 to 0.233, 0.252 and 0.243 in children and adolescents, adult females and adult males, respectively. Conclusions: The validated method was efficaciously applied to real finger and toe nails specimens from a population of males and females non GHB consumers. A preliminary cut-off of 5.0 ng/mg nail for endogenous GHB and 0.5 ng/mg for endogenous GHB-Gluc in the general population was proposed. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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16 pages, 2296 KiB  
Article
Optimization of Flavonoids Extraction Process in Panax notoginseng Stem Leaf and a Study of Antioxidant Activity and Its Effects on Mouse Melanoma B16 Cells
by Chun-Yan Dai, Peng-Fei Liu, Pei-Ran Liao, Yuan Qu, Cheng-Xiao Wang, Ye Yang and Xiu-Ming Cui
Molecules 2018, 23(9), 2219; https://doi.org/10.3390/molecules23092219 - 01 Sep 2018
Cited by 26 | Viewed by 4225
Abstract
The Panax notoginseng (P. notoginseng) stem leaf is rich in flavonoids. However, because of a lack of research on the flavonoid extraction process and functional development of P. notoginseng stem leaf, these parts are discarded as agricultural wastes. Therefore, in this [...] Read more.
The Panax notoginseng (P. notoginseng) stem leaf is rich in flavonoids. However, because of a lack of research on the flavonoid extraction process and functional development of P. notoginseng stem leaf, these parts are discarded as agricultural wastes. Therefore, in this study, we intend to optimize the extraction process and develop the skin-whitening functions of P. notoginseng stem leaf extracts. The extraction process of the stem and leaf of P. notoginseng flavonoid (SLPF) is optimized based on the Box–Behnken design (BBD) and the response surface methodology (RSM). The optimum extraction conditions of the SLPF are as follows: the extraction time, the ethanol concentration, the sodium dodecyl sulfate (SDS) content and the liquid material ratio (v/w, which are 52 min, 48.7%, 1.9%, and 20:1, respectively. Under the optimal extraction conditions, the average total SLPF content is 2.10%. The antioxidant activity and anti-deposition of melanin of mouse B16 cells of P. notoginseng stem leaf extracts are studied. The results indicate that the EC50 values of reducing activity, 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical scavenging activities, the superoxide anion removal ability, and the 2,2-azino-bis-3-ethylbenzthiazoline-6-sulphonic acid (ABTS) free radical removal ability are 7.212, 2.893, 2.949, and 0.855 mg/mL, respectively. The extracts IC50 values of the tyrosinase and melanin synthesis are 0.045 and 0.046 mg/mL, respectively. Therefore, the optimal processing technology for the SLPF obtained in this study not only increases its utilization rate, but also decreases material costs. The extracts from the P. notoginseng stem leaf may be developed as food or beauty products. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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10 pages, 2400 KiB  
Article
Development of a NIR Method for the In-Line Quantification of the Total Polyphenolic Content: A Study Applied on Ajuga genevensis L. Dry Extract Obtained in a Fluid Bed Process
by Alexandru Gavan, Liora Colobatiu, Andrei Mocan, Anca Toiu and Ioan Tomuta
Molecules 2018, 23(9), 2152; https://doi.org/10.3390/molecules23092152 - 27 Aug 2018
Cited by 5 | Viewed by 2993
Abstract
This study describes an innovative in-line near-infrared (NIR) process monitoring method for the quantification of the total polyphenolic content (TPC) of Ajuga genevensis dry extracts. The dry extract was obtained in a fluidized bed processor, by spraying and adsorbing a liquid extract onto [...] Read more.
This study describes an innovative in-line near-infrared (NIR) process monitoring method for the quantification of the total polyphenolic content (TPC) of Ajuga genevensis dry extracts. The dry extract was obtained in a fluidized bed processor, by spraying and adsorbing a liquid extract onto an inert powder support. NIR spectra were recorded continuously during the extract’s spraying process. For the calibration of the in-line TPC quantification method, samples were collected during the entire process. The TPC of each sample was assessed spectroscopically, by applying a UV-Vis reference method. The obtained values were further used in order to develop a quality OPLS prediction model by correlating them with the corresponding NIR spectra. The final dry extract registered good flowability and compressibility properties, a concentration in active principles three times higher than the one of the liquid extract and an overall process yield of 85%. The average TPC’s recovery of the NIR in-line prediction method, compared with the reference UV-Vis one, was 98.7%, indicating a reliable monitoring method which provided accurate predictions of the TPC during the process, permitting a good process overview and enabling us to establish the process’s end point at the exact moment when the product reaches the desired TPC concentration. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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22 pages, 2942 KiB  
Article
Insights into Tissue-specific Specialized Metabolism in Tieguanyin Tea Cultivar by Untargeted Metabolomics
by Si Chen, Jun Lin, Huihui Liu, Zhihong Gong, Xiaxia Wang, Meihong Li, Asaph Aharoni, Zhenbiao Yang and Xiaomin Yu
Molecules 2018, 23(7), 1817; https://doi.org/10.3390/molecules23071817 - 21 Jul 2018
Cited by 25 | Viewed by 6331
Abstract
Tea plants produce extremely diverse and abundant specialized metabolites, the types and levels of which are developmentally and environmentally regulated. However, little is known about how developmental cues affect the synthesis of many of these molecules. In this study, we conducted a comparative [...] Read more.
Tea plants produce extremely diverse and abundant specialized metabolites, the types and levels of which are developmentally and environmentally regulated. However, little is known about how developmental cues affect the synthesis of many of these molecules. In this study, we conducted a comparative profiling of specialized metabolites from six different tissues in a premium oolong tea cultivar, Tieguanyin, which is gaining worldwide popularity due to its uniquely rich flavors and health benefits. UPLC-QTOF MS combined with multivariate analyses tentatively identified 68 metabolites belonging to 11 metabolite classes, which exhibited sharp variations among tissues. Several metabolite classes, such as flavonoids, alkaloids, and hydroxycinnamic acid amides were detected predominantly in certain plant tissues. In particular, tricoumaroyl spermidine and dicoumaroyl putrescine were discovered as unique tea flower metabolites. This study offers novel insights into tissue-specific specialized metabolism in Tieguanyin, which provides a good reference point to explore gene-metabolite relationships in this cultivar. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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14 pages, 3958 KiB  
Article
Hydrophilic Interaction Liquid Chromatography-Electrospray Ionization Mass Spectrometry for Therapeutic Drug Monitoring of Metformin and Rosuvastatin in Human Plasma
by Nikolaos Antonopoulos, Giorgos Machairas, George Migias, Ariadni Vonaparti, Vasiliki Brakoulia, Constantinos Pistos, Dimitra Gennimata and Irene Panderi
Molecules 2018, 23(7), 1548; https://doi.org/10.3390/molecules23071548 - 27 Jun 2018
Cited by 12 | Viewed by 4675
Abstract
In this work a hydrophilic interaction liquid chromatography/positive ion electrospray mass spectrometric assay (HILIC/ESI-MS) has been developed and fully validated for the quantitation of metformin and rosuvastatin in human plasma. Sample preparation involved the use of 100 μL of human plasma, following protein [...] Read more.
In this work a hydrophilic interaction liquid chromatography/positive ion electrospray mass spectrometric assay (HILIC/ESI-MS) has been developed and fully validated for the quantitation of metformin and rosuvastatin in human plasma. Sample preparation involved the use of 100 μL of human plasma, following protein precipitation and filtration. Metformin, rosuvastatin and 4-[2-(propylamino) ethyl] indoline 2 one hydrochloride (internal standard) were separated by using an X-Bridge-HILIC BEH analytical column (150.0 × 2.1 mm i.d., particle size 3.5 μm) with isocratic elution. A mobile phase consisting of 12% (v/v) 15 mM ammonium formate water solution in acetonitrile was used for the separation and pumped at a flow rate of 0.25 mL min−1. The linear range of the assay was 100 to 5000 ng mL−1 and 2 to 100 ng mL−1 for metformin and rosuvastatin, respectively. The current HILIC-ESI/MS method allows for the accurate and precise quantitation of metformin and rosuvastatin in human plasma with a simple sample preparation and a short a chromatographic run time (less than 15 min). Plasma samples from eight patients were further analysed proving the capability of the proposed method to support a wide range of clinical studies. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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18 pages, 2949 KiB  
Article
Production of Minor Ginenosides from Panax notoginseng by Microwave Processing Method and Evaluation of Their Blood-Enriching and Hemostatic Activity
by Huiying Liu, Jun Pan, Ye Yang, Xiuming Cui and Yuan Qu
Molecules 2018, 23(6), 1243; https://doi.org/10.3390/molecules23061243 - 23 May 2018
Cited by 12 | Viewed by 3103
Abstract
A green solvent extraction technology involving a microwave processing method was used to increase the content of minor ginsenosides from Panax notoginseng. This article aims to investigate the optimization of preparation of the minor ginsenosides by this microwave processing method using single-factor [...] Read more.
A green solvent extraction technology involving a microwave processing method was used to increase the content of minor ginsenosides from Panax notoginseng. This article aims to investigate the optimization of preparation of the minor ginsenosides by this microwave processing method using single-factor experiments and response surface methodology (RSM), and discuss the blood-enriching activity and hemostatic activity of the extract of microwave processed P. notoginseng (EMPN) The RSM for production of the minor ginsenosides was based on a three-factor and three-level Box-Behnken design. When the optimum conditions of microwave power, temperature and time were 495.03 W, 150.68 °C and 20.32 min, respectively, results predicted that the yield of total minor ginsenosides (Y9) would be 93.13%. The actual value of Y9 was very similar to the predicted value. In addition, the pharmacological results of EMPN in vivo showed that EMPN had the effect of enriching blood in N-acetylphenylhydrazine (APH) and cyclophosphamide (CTX)-induced blood deficient mice because of the increasing content of white blood cells (WBCs) and hemoglobin (HGB) in blood. Hemostatic activity in vitro of EMPN showed that it had significantly shortened the clotting time in PT testing (p < 0.05). The hemostatic effect of EMPN was mainly caused by its components of Rh4, 20(S)-Rg3 and 20(R)-Rg3. This microwave processing method is simple and suitable to mass-produce the minor ginsenosides from P. notoginseng. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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22 pages, 6004 KiB  
Article
Optimisation of Ethanol-Reflux Extraction of Saponins from Steamed Panax notoginseng by Response Surface Methodology and Evaluation of Hematopoiesis Effect
by Yupiao Hu, Xiuming Cui, Zejun Zhang, Lijuan Chen, Yiming Zhang, Chengxiao Wang, Xiaoyan Yang, Yuan Qu and Yin Xiong
Molecules 2018, 23(5), 1206; https://doi.org/10.3390/molecules23051206 - 17 May 2018
Cited by 26 | Viewed by 4187
Abstract
The present study aims to optimize the ethanol-reflux extraction conditions for extracting saponins from steamed Panax notoginseng (SPN). Four variables including the extraction time (0.5–2.5 h), ethanol concentration (50–90%), water to solid ratio (W/S, 8–16), and times of extraction (1–5) were investigated by [...] Read more.
The present study aims to optimize the ethanol-reflux extraction conditions for extracting saponins from steamed Panax notoginseng (SPN). Four variables including the extraction time (0.5–2.5 h), ethanol concentration (50–90%), water to solid ratio (W/S, 8–16), and times of extraction (1–5) were investigated by using the Box-Behnken design response surface methodology (BBD-RSM). For each response, a second-order polynomial model with high R2 values (>0.9690) was developed using multiple linear regression analysis and the optimum conditions to maximize the yield (31.96%), content (70.49 mg/g), and antioxidant activity (EC50 value of 0.0421 mg/mL) for saponins extracted from SPN were obtained with a extraction time of 1.51 h, ethanol concentration of 60%, extraction done 3 times, and a W/S of 10. The experimental values were in good consistency with the predicted ones. In addition, the extracted SPN saponins could significantly increase the levels of blood routine parameters compared with the model group (p < 0.01) and there was no significant difference in the hematopoiesis effect between the SPN group and the SPN saponins group, of which the dose was 15 times lower than the former one. It is suggested that the SPN saponins extracted by the optimized method had similar functions of “blood tonifying” at a much lower dose. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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16 pages, 3677 KiB  
Article
Compounds Identification in Semen Cuscutae by Ultra-High-Performance Liquid Chromatography (UPLCs) Coupled to Electrospray Ionization Mass Spectrometry
by Ying Zhang, Hui Xiong, Xinfang Xu, Xue Xue, Mengnan Liu, Shuya Xu, Huan Liu, Yan Gao, Hui Zhang and Xiangri Li
Molecules 2018, 23(5), 1199; https://doi.org/10.3390/molecules23051199 - 17 May 2018
Cited by 38 | Viewed by 6762
Abstract
Semen Cuscutae is commonly used in traditional Chinese medicine and contains a series of compounds such as flavonoids, chlorogenic acids and lignans. In this study, we identified different kinds of compositions by ultra-high-performance liquid chromatography (UPLC) coupled to electrospray ionization mass spectrometry (MS). [...] Read more.
Semen Cuscutae is commonly used in traditional Chinese medicine and contains a series of compounds such as flavonoids, chlorogenic acids and lignans. In this study, we identified different kinds of compositions by ultra-high-performance liquid chromatography (UPLC) coupled to electrospray ionization mass spectrometry (MS). A total of 45 compounds were observed, including 20 chlorogenic acids, 23 flavonoids and 2 lignans. 23 of them are reported for the first time including 6-O-caffeoyl-β-glucose, 3-O-(4′-O-Caffeoylglucosyl) quinic acid, etc. Their structures were established by retention behavior, extensive analyses of their MS spectra and further determined by comparison of their MS data with those reported in the literature. As chlorogenic acids and flavonoids are phenolic compounds that are predominant in Semen Cuscutae, in conclusion, phenolic compounds are the major constituents of Semen Cuscutae. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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17 pages, 1757 KiB  
Article
Effects of Ultrasound Assisted Extraction in Conjugation with Aid of Actinidin on the Molecular and Physicochemical Properties of Bovine Hide Gelatin
by Tanbir Ahmad, Amin Ismail, Siti A. Ahmad, Khalilah A. Khalil, Teik K. Leo, Elmutaz A. Awad, Jurhamid C. Imlan and Awis Q. Sazili
Molecules 2018, 23(4), 730; https://doi.org/10.3390/molecules23040730 - 22 Mar 2018
Cited by 23 | Viewed by 5638
Abstract
Actinidin was used to pretreat the bovine hide and ultrasonic wave (53 kHz and 500 W) was used for the time durations of 2, 4 and 6 h at 60 °C to extract gelatin samples (UA2, UA4 and UA6, respectively). Control (UAC) gelatin [...] Read more.
Actinidin was used to pretreat the bovine hide and ultrasonic wave (53 kHz and 500 W) was used for the time durations of 2, 4 and 6 h at 60 °C to extract gelatin samples (UA2, UA4 and UA6, respectively). Control (UAC) gelatin was extracted using ultrasound for 6 h at 60 °C without enzyme pretreatment. There was significant (p < 0.05) increase in gelatin yield as the time duration of ultrasound treatment increased with UA6 giving the highest yield of 19.65%. Gel strength and viscosity of UAC and UA6 extracted gelatin samples were 627.53 and 502.16 g and 16.33 and 15.60 mPa.s, respectively. Longer duration of ultrasound treatment increased amino acids content of the extracted gelatin and UAC exhibited the highest content of amino acids. Progressive degradation of polypeptide chains was observed in the protein pattern of the extracted gelatin as the time duration of ultrasound extraction increased. Fourier transform infrared (FTIR) spectroscopy depicted loss of molecular order and degradation in UA6. Scanning electron microscopy (SEM) revealed protein aggregation and network formation in the gelatin samples with increasing time of ultrasound treatment. The study indicated that ultrasound assisted gelatin extraction using actinidin exhibited high yield with good quality gelatin. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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10 pages, 3648 KiB  
Article
Modification and Characterization of Fe3O4 Nanoparticles for Use in Adsorption of Alkaloids
by Linyan Yang, Jing Tian, Jiali Meng, Ruili Zhao, Cun Li, Jifei Ma and Tianming Jin
Molecules 2018, 23(3), 562; https://doi.org/10.3390/molecules23030562 - 02 Mar 2018
Cited by 67 | Viewed by 4579
Abstract
Magnetite (Fe3O4) is a ferromagnetic iron oxide of both Fe(II) and Fe(III), prepared by FeCl2 and FeCl3. XRD was used for the confirmation of Fe3O4. Via the modification of Tetraethyl orthosilicate (TEOS), [...] Read more.
Magnetite (Fe3O4) is a ferromagnetic iron oxide of both Fe(II) and Fe(III), prepared by FeCl2 and FeCl3. XRD was used for the confirmation of Fe3O4. Via the modification of Tetraethyl orthosilicate (TEOS), (3-Aminopropyl)trimethoxysilane (APTMS), and Alginate (AA), Fe3O4@SiO2, Fe3O4@SiO2-NH2, and Fe3O4@SiO2-NH2-AA nanoparticles could be obtained, and IR and SEM were used for the characterizations. Alkaloid adsorption experiments exhibited that, as for Palmatine and Berberine, the most adsorption could be obtained at pH 8 when the adsorption time was 6 min. The adsorption percentage of Palmatine was 22.2%, and the adsorption percentage of Berberine was 23.6% at pH 8. Considering the effect of adsorption time on liquid phase system, the adsorption conditions of 8 min has been chosen when pH 7 was used. The adsorption percentage of Palmatine was 8.67%, and the adsorption percentage of Berberine was 7.25%. Considering the above conditions, pH 8 and the adsorption time of 8min could be chosen for further uses. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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10 pages, 961 KiB  
Article
Isolation and Purification of Two Isoflavones from Hericium erinaceum Mycelium by High-Speed Counter-Current Chromatography
by Jinzhe He, Peng Fan, Simin Feng, Ping Shao and Peilong Sun
Molecules 2018, 23(3), 560; https://doi.org/10.3390/molecules23030560 - 02 Mar 2018
Cited by 18 | Viewed by 3961
Abstract
High-speed counter-current chromatography (HSCCC) was used to separate and purify two isoflavones for the first time from Hericium erinaceum (H. erinaceum) mycelium using a two-phase solvent system composed of chloroform-dichloromethane-methanol-water (4:2:3:2, v/v/v/v). These two [...] Read more.
High-speed counter-current chromatography (HSCCC) was used to separate and purify two isoflavones for the first time from Hericium erinaceum (H. erinaceum) mycelium using a two-phase solvent system composed of chloroform-dichloromethane-methanol-water (4:2:3:2, v/v/v/v). These two isoflavones were identified as genistein (4′,5,7-trihydroxyisoflavone, C15H10O5) and daidzein (4′,7-dihydroxyisoflavone, C15H10O4), using infrared spectroscopy (IR), electro-spary ionisation mass (ESI-MS), 1H-nuclear magnetic resonance (NMR) and 13C-NMR spectra. About 23 mg genistein with 95.7% purity and 18 mg daidzein with 97.3% purity were isolated from 150 mg ethanolic extract of H. erinaceum mycelium. The results demonstrated that HSCCC was a feasible method to separate and purify genistein and daidzein from H. erinaceum mycelium. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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13 pages, 3320 KiB  
Article
Fast Determination of Yttrium and Rare Earth Elements in Seawater by Inductively Coupled Plasma-Mass Spectrometry after Online Flow Injection Pretreatment
by Zuhao Zhu and Airong Zheng
Molecules 2018, 23(2), 489; https://doi.org/10.3390/molecules23020489 - 23 Feb 2018
Cited by 26 | Viewed by 4795
Abstract
A method for daily monitoring of yttrium and rare earth elements (YREEs) in seawater using a cheap flow injection system online coupled to inductively coupled plasma-mass spectrometry is reported. Toyopearl AF Chelate 650M® resin permits separation and concentration of YREEs using a [...] Read more.
A method for daily monitoring of yttrium and rare earth elements (YREEs) in seawater using a cheap flow injection system online coupled to inductively coupled plasma-mass spectrometry is reported. Toyopearl AF Chelate 650M® resin permits separation and concentration of YREEs using a simple external calibration. A running cycle consumed 6 mL sample and took 5.3 min, providing a throughput of 11 samples per hour. Linear ranges were up to 200 ng kg−1 except Tm (100 ng kg−1). The precision of the method was <6% (RSDs, n = 5), and recoveries ranged from 93% to 106%. Limits of detection (LODs) were in the range 0.002 ng kg−1 (Tm) to 0.078 ng kg−1 (Ce). Good agreement between YREEs concentrations in CASS-4 and SLEW-3 obtained in this work and results from other studies was observed. The proposed method was applied to the determination of YREEs in seawater from the Jiulong River Estuary and the Taiwan Strait. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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11 pages, 1350 KiB  
Article
Qualitative and Quantitative Phytochemical Analysis of Different Extracts from Thymus algeriensis Aerial Parts
by Nassima Boutaoui, Lahcene Zaiter, Fadila Benayache, Samir Benayache, Simone Carradori, Stefania Cesa, Anna Maria Giusti, Cristina Campestre, Luigi Menghini, Denise Innosa and Marcello Locatelli
Molecules 2018, 23(2), 463; https://doi.org/10.3390/molecules23020463 - 20 Feb 2018
Cited by 28 | Viewed by 4828
Abstract
This study was performed to evaluate the metabolite recovery from different extraction methods applied to Thymus algeriensis aerial parts. A high-performance liquid chromatographic method using photodiode array detector with gradient elution has been developed and validated for the simultaneous estimation of different phenolic [...] Read more.
This study was performed to evaluate the metabolite recovery from different extraction methods applied to Thymus algeriensis aerial parts. A high-performance liquid chromatographic method using photodiode array detector with gradient elution has been developed and validated for the simultaneous estimation of different phenolic compounds in the extracts and in their corresponding purified fractions. The experimental results show that microwave-assisted aqueous extraction for 15 min at 100 °C gave the most phenolics-enriched extract, reducing extraction time without degradation effects on bioactives. Sixteen compounds were identified in this extract, 11 phenolic compounds and five flavonoids, all known for their biological activities. Color analysis and determination of chlorophylls and carotenoids implemented the knowledge of the chemical profile of this plant. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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14 pages, 262 KiB  
Article
A Comparative Assessment of Biological Effects and Chemical Profile of Italian Asphodeline lutea Extracts
by Dora Melucci, Marcello Locatelli, Clinio Locatelli, Alessandro Zappi, Francesco De Laurentiis, Simone Carradori, Cristina Campestre, Lidia Leporini, Gokhan Zengin, Carene Marie Nancy Picot, Luigi Menghini and Mohamad Fawzi Mahomoodally
Molecules 2018, 23(2), 461; https://doi.org/10.3390/molecules23020461 - 19 Feb 2018
Cited by 22 | Viewed by 3757
Abstract
The present study aims to highlight the therapeutic potential of Asphodeline lutea (AL), a wild edible plant of the Mediterranean diet. Roots, aerial parts, and flowers of AL at two different phenological stages were collected from three locations in Italy. The [...] Read more.
The present study aims to highlight the therapeutic potential of Asphodeline lutea (AL), a wild edible plant of the Mediterranean diet. Roots, aerial parts, and flowers of AL at two different phenological stages were collected from three locations in Italy. The inhibitory activities of extracts on strategic enzymes linked to human diseases were assessed. The antioxidant properties were evaluated in vitro, using six standard bioassays. The phenolic and anthraquinone profiles were also established using HPLC-PDA. Zinc, cadmium, lead, and copper contents were also determined. All the samples inhibited acetylcholinesterase (from 1.51 to 2.20 mg GALAEs/g extract), tyrosinase (from 7.50 to 25.3 mg KAEs/g extract), and α-amylase (from 0.37 to 0.51 mmol ACAEs/g extract). Aloe-emodin and physcion were present in all parts, while rhein was not detected. The phenolic profile and the heavy metals composition of specimens gathered from three different regions of Italy were different. It can be argued that samples collected near the street can contain higher concentrations of heavy metals. The experimental data confirm that the A. lutea species could be considered as a potential source of bioactive metabolites, and its consumption could play a positive and safe role in human health maintenance. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
7 pages, 1181 KiB  
Article
A Novel Flavonoid Glucoside from the Fruits of Lycium ruthenicun
by Jing-Jing Qi, Yong-Ming Yan, Li-Zhi Cheng, Bao-Hua Liu, Fu-Ying Qin and Yong-Xian Cheng
Molecules 2018, 23(2), 325; https://doi.org/10.3390/molecules23020325 - 03 Feb 2018
Cited by 12 | Viewed by 3752
Abstract
A novel flavonoid glucoside, ruthenicunoid A (1), together with eight known substances, were isolated from the fruits of Lycium ruthenicun Murr. Their structures were elucidated by extensive spectroscopic data and chemical methods. Especially, the absolute configuration of glucose residue in 1 [...] Read more.
A novel flavonoid glucoside, ruthenicunoid A (1), together with eight known substances, were isolated from the fruits of Lycium ruthenicun Murr. Their structures were elucidated by extensive spectroscopic data and chemical methods. Especially, the absolute configuration of glucose residue in 1 was assigned by acid hydrolysis followed by derivatization and GC analysis. Biological evaluation towards Sirtuin 1 (SIRT1) found that compounds 1 and 2 exhibit inhibitory activity against SIRT1 in a concentration-dependent manner, indicating its potential on SIRT1-associated disorders. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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18 pages, 1805 KiB  
Article
Metabolite Profiling of 14 Wuyi Rock Tea Cultivars Using UPLC-QTOF MS and UPLC-QqQ MS Combined with Chemometrics
by Si Chen, Meihong Li, Gongyu Zheng, Tingting Wang, Jun Lin, Shanshan Wang, Xiaxia Wang, Qianlin Chao, Shixian Cao, Zhenbiao Yang and Xiaomin Yu
Molecules 2018, 23(2), 104; https://doi.org/10.3390/molecules23020104 - 24 Jan 2018
Cited by 89 | Viewed by 9006
Abstract
Wuyi Rock tea, well-recognized for rich flavor and long-lasting fragrance, is a premium subcategory of oolong tea mainly produced in Wuyi Mountain and nearby regions of China. The quality of tea is mainly determined by the chemical constituents in the tea leaves. However, [...] Read more.
Wuyi Rock tea, well-recognized for rich flavor and long-lasting fragrance, is a premium subcategory of oolong tea mainly produced in Wuyi Mountain and nearby regions of China. The quality of tea is mainly determined by the chemical constituents in the tea leaves. However, this remains underexplored for Wuyi Rock tea cultivars. In this study, we investigated the leaf metabolite profiles of 14 major Wuyi Rock tea cultivars grown in the same producing region using UPLC-QTOF MS and UPLC-QqQ MS with data processing via principal component analysis and cluster analysis. Relative quantitation of 49 major metabolites including flavan-3-ols, proanthocyanidins, flavonol glycosides, flavone glycosides, flavonone glycosides, phenolic acid derivatives, hydrolysable tannins, alkaloids and amino acids revealed clear variations between tea cultivars. In particular, catechins, kaempferol and quercetin derivatives were key metabolites responsible for cultivar discrimination. Information on the varietal differences in the levels of bioactive/functional metabolites, such as methylated catechins, flavonol glycosides and theanine, offers valuable insights to further explore the nutritional values and sensory qualities of Wuyi Rock tea. It also provides potential markers for tea plant fingerprinting and cultivar identification. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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10 pages, 801 KiB  
Article
Characterization of Odors of Wood by Gas Chromatography-Olfactometry with Removal of Extractives as Attempt to Control Indoor Air Quality
by Ru Liu, Chen Wang, Anmin Huang and Bin Lv
Molecules 2018, 23(1), 203; https://doi.org/10.3390/molecules23010203 - 18 Jan 2018
Cited by 32 | Viewed by 6393
Abstract
Indoor air quality problems are usually revealed by occupants’ complaints. In this study, the odors of two types of hardwood species, namely, Cathy poplar (Populus cathayana Rehd.) and rubberwood (Hevea brasiliensis) were selected and extracted with ethanol-toluene for removal of [...] Read more.
Indoor air quality problems are usually revealed by occupants’ complaints. In this study, the odors of two types of hardwood species, namely, Cathy poplar (Populus cathayana Rehd.) and rubberwood (Hevea brasiliensis) were selected and extracted with ethanol-toluene for removal of extractives in an attempt to eliminate the odors. The odorous components of neat and extracted woods were identified by gas chromatography-mass spectrometry/olfactometry (GC-MS/O). The results showed that about 33 kinds of key volatile compounds (peak area above 0.2%) were detected from the GC-MS, and about 40 kinds of odorants were identified from GC-O. The components were concentrated between 15 and 33 min in GC-O, which was different from the concentration time in GC-MS. Lots of the odors identified from GC-O were unpleasant to humans, and variously described as stinky, burnt, leather, bug, herb, etc. These odors may originate from the thermos-oxidation of wood components. After extraction, the amounts and intensities of some odorants decreased, while some remained. However, the extraction process resulted in a benzene residue and led to increased benzene odor. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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12 pages, 2373 KiB  
Article
Determination of Branched-Chain Keto Acids in Serum and Muscles Using High Performance Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometry
by You Zhang, Bingjie Yin, Runxian Li and Pingli He
Molecules 2018, 23(1), 147; https://doi.org/10.3390/molecules23010147 - 11 Jan 2018
Cited by 9 | Viewed by 5234
Abstract
Branched-chain keto acids (BCKAs) are derivatives from the first step in the metabolism of branched-chain amino acids (BCAAs) and can provide important information on animal health and disease. Here, a simple, reliable and effective method was developed for the determination of three BCKAs [...] Read more.
Branched-chain keto acids (BCKAs) are derivatives from the first step in the metabolism of branched-chain amino acids (BCAAs) and can provide important information on animal health and disease. Here, a simple, reliable and effective method was developed for the determination of three BCKAs (α-ketoisocaproate, α-keto-β-methylvalerate and α-ketoisovalerate) in serum and muscle samples using high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (HPLC-Q-TOF/MS). The samples were extracted using methanol and separated on a 1.8 μm Eclipse Plus C18 column within 10 min. The mobile phase was 10 mmol L−1 ammonium acetate aqueous solution and acetonitrile. The results showed that recoveries for the three BCKAs ranged from 78.4% to 114.3% with relative standard deviation (RSD) less than 9.7%. The limit of quantitation (LOQ) were 0.06~0.23 μmol L−1 and 0.09~0.27 nmol g−1 for serum and muscle samples, respectively. The proposed method can be applied to the determination of three BCKAs in animal serum and muscle samples. Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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Review

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12 pages, 708 KiB  
Review
Recent Advances in Applications of Ionic Liquids in Miniaturized Microextraction Techniques
by Maria Kissoudi and Victoria Samanidou
Molecules 2018, 23(6), 1437; https://doi.org/10.3390/molecules23061437 - 13 Jun 2018
Cited by 63 | Viewed by 4593
Abstract
Green sample preparation is one of the most challenging aspects in green analytical chemistry. In this framework, miniaturized microextraction techniques have been developed and are widely performed due to their numerous positive features such as simplicity, limited need for organic solvents, instrumentation of [...] Read more.
Green sample preparation is one of the most challenging aspects in green analytical chemistry. In this framework, miniaturized microextraction techniques have been developed and are widely performed due to their numerous positive features such as simplicity, limited need for organic solvents, instrumentation of low cost and short time of extraction. Also, ionic liquids (ILs) have unequivocally a “green” character, which they owe to their unique properties including the re-usage, the high reaction efficiency and selectivity in room temperature, the ability to dissolve both organic and inorganic compounds, and thermal stability. In the present review, the recent advances in the application of ionic liquids in miniaturized liquid and solid phase extraction techniques as extractants, intermediate solvents, mediators and desorption solvents are discussed, quoting the advantages and drawbacks of each individual technique. Some of the most important sample preparation techniques covered include solid-phase microextraction (SPME), dispersive liquid-liquid microextraction (DLLME), single-drop microextraction (SDME), stir bar sorptive extraction (SBSE), and stir cake sorptive extraction (SCSE). Full article
(This article belongs to the Special Issue Innovative Extraction Techniques and Hyphenated Instrument Configuration for Complex Matrices Analysis)
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