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14 pages, 2224 KiB

Open AccessArticle

One-Pot Production of RNA in High Yield and Purity Through Cleaving Tandem Transcripts

by Hannes Feyrer, Raluca Munteanu, Lorenzo Baronti and Katja Petzold

Molecules 2020, 25(5), 1142; https://doi.org/10.3390/molecules25051142 - 4 Mar 2020

Cited by 13 | Viewed by 5904

Abstract

There is an increasing demand for efficient and robust production of short RNA molecules in both pharmaceutics and research. A standard method is in vitro transcription by T7 RNA polymerase. This method is sequence-dependent on efficiency and is limited to products longer than [...] Read more.

There is an increasing demand for efficient and robust production of short RNA molecules in both pharmaceutics and research. A standard method is in vitro transcription by T7 RNA polymerase. This method is sequence-dependent on efficiency and is limited to products longer than ~12 nucleotides. Additionally, the native initiation sequence is required to achieve high yields, putting a strain on sequence variability. Deviations from this sequence can lead to side products, requiring laborious purification, further decreasing yield. We here present transcribing tandem repeats of the target RNA sequence followed by site-specific cleavage to obtain RNA in high purity and yield. This approach makes use of a plasmid DNA template and RNase H-directed cleavage of the transcript. The method is simpler and faster than previous protocols, as it can be performed as one pot synthesis and provides at the same time higher yields of RNA. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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13 pages, 1538 KiB

Open AccessArticle

Poly (Octadecyl Methacrylate-Co-Trimethylolpropane Trimethacrylate) Monolithic Column for Hydrophobic in-Tube Solid-Phase Microextraction of Chlorophenoxy Acid Herbicides

by Wenbang Li, Fangling Wu, Yongwei Dai, Jing Zhang, Bichen Ni and Jiabin Wang

Molecules 2019, 24(9), 1678; https://doi.org/10.3390/molecules24091678 - 29 Apr 2019

Cited by 14 | Viewed by 2987

Abstract

Chlorophenoxy acid herbicides (CAHs), which are widely used on cereal crops, have become an important pollution source in grains. In this work, a highly hydrophobic poly (octadecyl methacrylate-co-trimethylolpropane trimethacrylate) [poly (OMA-co-TRIM)] monolithic column has been specially prepared for hydrophobic in-tube solid-phase microextraction (SPME) [...] Read more.

Chlorophenoxy acid herbicides (CAHs), which are widely used on cereal crops, have become an important pollution source in grains. In this work, a highly hydrophobic poly (octadecyl methacrylate-co-trimethylolpropane trimethacrylate) [poly (OMA-co-TRIM)] monolithic column has been specially prepared for hydrophobic in-tube solid-phase microextraction (SPME) of CAHs in rice grains. Due to the hydrophobicity of CAHs in acid conditions, trace CAHs could be efficiently extracted by the prepared monolith with strong hydrophobic interaction. Several factors for online hydrophobic in-tube SPME, including the length of the monolithic column, ACN and trifluoroacetic acid percentage in the sampling solution, elution volume, and elution flow rate, were investigated with respect to the extraction efficiencies of CAHs. Under the optimized conditions, the limits of detection of the four CAHs fell in the range of 0.9–2.1 μg/kg. The calibration curves provided a wide linear range of 5–600 μg/kg and showed good linearity. The recoveries of this method ranged from 87.3% to 111.6%, with relative standard deviations less than 7.3%. Using this novel, highly hydrophobic poly (OMA-co-TRIM) monolith as sorbent, a simple and sensitive online in-tube SPME-HPLC method was proposed for analysis of CAHs residue in practical samples of rice grains. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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12 pages, 1293 KiB

Open AccessArticle

Determination of Barbiturates in Biological Specimens by Flat Membrane-Based Liquid-Phase Microextraction and Liquid Chromatography-Mass Spectrometry

by Ruiqin Zhu, Ying Dong, Xiangyang Cai and Chuixiu Huang

Molecules 2019, 24(8), 1494; https://doi.org/10.3390/molecules24081494 - 16 Apr 2019

Cited by 14 | Viewed by 5712

Abstract

The wide abuse of barbiturates has aroused extensive public concern. Therefore, the determination of such drugs is becoming essential in therapeutic drug monitoring and forensic science. Herein, a simple, efficient, and inexpensive sample preparation technique, namely, flat membrane-based liquid-phase microextraction (FM-LPME) followed by [...] Read more.

The wide abuse of barbiturates has aroused extensive public concern. Therefore, the determination of such drugs is becoming essential in therapeutic drug monitoring and forensic science. Herein, a simple, efficient, and inexpensive sample preparation technique, namely, flat membrane-based liquid-phase microextraction (FM-LPME) followed by liquid chromatography-mass spectrometry (LC-MS), was used to determine barbiturates in biological specimens. Factors that may influence the efficiency including organic extraction solvent, pH, and composition of donor and acceptor phases, extraction time, and salt addition to the sample (donor phase) were investigated and optimized. Under the optimized extraction conditions, the linear ranges of the proposed FM-LPME/LC-MS method (with correlation coefficient factors ≥ 0.99) were 7.5–750 ng mL⁻¹ for whole blood, 5.0–500 ng mL⁻¹ for urine, and 25–2500 ng g⁻¹ for liver. Repeatability between 5.0 and 13.7% was obtained and the limit of detection (LOD) values ranged from 1.5 to 3.1 ng mL⁻¹, from 0.6 to 3.6 ng mL⁻¹, and from 5.2 to 10.0 ng g⁻¹ for whole blood, urine, and liver samples, respectively. This method was successfully applied for the analysis of barbiturates in blood and liver from rats treated with these drugs, and excellent sample cleanup was achieved. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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13 pages, 2848 KiB

Open AccessArticle

Primary Step Towards In Situ Detection of Chemical Biomarkers in the UNIVERSE via Liquid-Based Analytical System: Development of an Automated Online Trapping/Liquid Chromatography System

by Thomas Ribette, Bertrand Leroux, Balkis Eddhif, Audrey Allavena, Marc David, Robert Sternberg, Pauline Poinot and Claude Geffroy-Rodier

Molecules 2019, 24(7), 1429; https://doi.org/10.3390/molecules24071429 - 11 Apr 2019

Cited by 3 | Viewed by 3149

Abstract

The search for biomarkers in our solar system is a fundamental challenge for the space research community. It encompasses major difficulties linked to their very low concentration levels, their ambiguous origins (biotic or abiotic), as well as their diversity and complexity. Even if, [...] Read more.

The search for biomarkers in our solar system is a fundamental challenge for the space research community. It encompasses major difficulties linked to their very low concentration levels, their ambiguous origins (biotic or abiotic), as well as their diversity and complexity. Even if, in 40 years’ time, great improvements in sample pre-treatment, chromatographic separation and mass spectrometry detection have been achieved, there is still a need for new in situ scientific instrumentation. This work presents an original liquid chromatographic system with a trapping unit dedicated to the one-pot detection of a large set of non-volatile extra-terrestrial compounds. It is composed of two units, monitored by a single pump. The first unit is an online trapping unit able to trap polar, apolar, monomeric and polymeric organics. The second unit is an online analytical unit with a high-resolution Q-Orbitrap mass spectrometer. The designed single pump system was as efficient as a laboratory dual-trap LC system for the analysis of amino acids, nucleobases and oligopeptides. The overall setup significantly improves sensitivity, providing limits of detection ranging from ppb to ppt levels, thus meeting with in situ enquiries. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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15 pages, 1257 KiB

Open AccessArticle

High Flow-Rate Sample Loading in Large Volume Whole Water Organic Trace Analysis Using Positive Pressure and Finely Ground Sand as a SPE-Column In-Line Filter

by Ola Svahn and Erland Björklund

Molecules 2019, 24(7), 1426; https://doi.org/10.3390/molecules24071426 - 11 Apr 2019

Cited by 16 | Viewed by 3803

Abstract

By using an innovative, positive pressure sample loading technique in combination with an in-line filter of finely ground sand the bottleneck of solid phase extraction (SPE) can be reduced. Recently published work by us has shown the proof of concept of the technique. [...] Read more.

By using an innovative, positive pressure sample loading technique in combination with an in-line filter of finely ground sand the bottleneck of solid phase extraction (SPE) can be reduced. Recently published work by us has shown the proof of concept of the technique. In this work, emphasis is put on the SPE flow rate and method validation for 26 compounds of emerging environmental concern, mainly from the 1st and 2nd EU Watch List, with various physicochemical properties. The mean absolute recoveries in % and relative standard deviations (RSD) in % for the investigated compounds from spiked pure water samples at the three investigated flow rates of 10, 20, and 40 mL/min were 63.2% (3.2%), 66.9% (3.3%), and 69.0% (4.0%), respectively. All three flow rates produced highly repeatable results, and this allowed a flow rate increase of up to 40 mL/min for a 200 mg, 6 mL, reversed phase SPE cartridge without compromising the recoveries. This figure is more than four times the maximum flow rate recommended by manufacturers. It was indicated that some compounds, especially pronounced for the investigated macrolide molecules, might suffer when long contact times with the sample glass bottle occurs. A reduced contact time somewhat decreases this complication. A very good repeatability also held true for experiments on both spiked matrix-rich pond water (high and low concentrations) and recipient waters (river and wastewater) applying 40 mL/min. This work has shown that, for a large number of compounds of widely differing physicochemical properties, there is a generous flow rate window from 10 to 40 mL/min where sample loading can be conducted. A sample volume of 0.5 L, which at the recommended maximum flow rate speed of 10 mL/min, would previously take 50 min, can now be processed in 12 min using a flow rate of 40 mL/min. This saves 38 min per processed sample. This low-cost technology allows the sample to be transferred to the SPE-column, closer to the sample location and by the person taking the sample. This further means that only the sample cartridge would need to be sent to the laboratory, instead of the whole water sample, like today’s procedure. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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13 pages, 2065 KiB

Open AccessArticle

Solvent Front Position Extraction with Semi-Automatic Device as a Powerful Sample Preparation Procedure Prior to Quantitative Instrumental Analysis

by Anna Klimek-Turek, Kamila Jaglińska, Magdalena Imbierowicz and Tadeusz Henryk Dzido

Molecules 2019, 24(7), 1358; https://doi.org/10.3390/molecules24071358 - 6 Apr 2019

Cited by 15 | Viewed by 3018

Abstract

The new prototype device is applied to the Solvent Front Position Extraction (SFPE) sample preparation procedure. The mobile phase is deposited onto the chromatographic plate adsorbent layer by the pipette, which is moved, according to programmed movement path, by a 3D printer mechanism. [...] Read more.

The new prototype device is applied to the Solvent Front Position Extraction (SFPE) sample preparation procedure. The mobile phase is deposited onto the chromatographic plate adsorbent layer by the pipette, which is moved, according to programmed movement path, by a 3D printer mechanism. The application of the prototype device to SFPE procedure leads to the increased repeatability of the results and significant reduction of the analysis time in comparison to the classical procedure of chromatogram development. Additionally, the new equipment allows use procedures that are not possible to run using the classic chromatogram development. In this paper, the results of manual and semi-automatic sample preparation with SFPE are compared and the possible application of this prototype device is discussed. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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10 pages, 2234 KiB

Open AccessArticle

A Sample Preparation Technique Using Biocompatible Composites for Biomedical Applications

by Huifang Liu, Geun Su Noh, Yange Luan, Zhen Qiao, Bonhan Koo, Yoon Ok Jang and Yong Shin

Molecules 2019, 24(7), 1321; https://doi.org/10.3390/molecules24071321 - 3 Apr 2019

Cited by 7 | Viewed by 2826

Abstract

Infectious diseases, especially pathogenic infections, are a growing threat to public health worldwide. Since pathogenic bacteria usually exist in complex matrices at very low concentrations, the development of technology for rapid, convenient, and biocompatible sample enrichment is essential for sensitive diagnostics. In this [...] Read more.

Infectious diseases, especially pathogenic infections, are a growing threat to public health worldwide. Since pathogenic bacteria usually exist in complex matrices at very low concentrations, the development of technology for rapid, convenient, and biocompatible sample enrichment is essential for sensitive diagnostics. In this study, a cucurbit[6]uril (CB) supermolecular decorated amine-functionalized diatom (DA) composite was fabricated to support efficient sample enrichment and in situ nucleic acid preparation from enriched pathogens and cells. CB was introduced to enhance the rate and effectiveness of pathogen absorption using the CB–DA composite. This novel CB–DA composite achieved a capture efficiency of approximately 90% at an Escherichia coli concentration of 10⁶ CFU/mL within 3 min. Real-time PCR analyses of DNA samples recovered using the CB–DA enrichment system showed a four-fold increase in the early amplification signal strength, and this effective method for capturing nucleic acid might be useful for preparing samples for diagnostic systems. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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14 pages, 3662 KiB

Open AccessArticle

New Vortex-Synchronized Matrix Solid-Phase Dispersion Method for Simultaneous Determination of Four Anthraquinones in Cassiae Semen

by Luyi Jiang, Jie Wang, Huan Zhang, Caijing Liu, Yiping Tang and Chu Chu

Molecules 2019, 24(7), 1312; https://doi.org/10.3390/molecules24071312 - 3 Apr 2019

Cited by 15 | Viewed by 2838

Abstract

In this study, a green ionic-liquid based vortex-synchronized matrix solid-phase dispersion (VS-MSPD) combined with high performance liquid chromatography (HPLC) method was developed as a quantitative determination method for four anthraquinones in Cassiae Semen. Two conventional adsorbents, C₁₈ and silica gel were investigated. [...] Read more.

In this study, a green ionic-liquid based vortex-synchronized matrix solid-phase dispersion (VS-MSPD) combined with high performance liquid chromatography (HPLC) method was developed as a quantitative determination method for four anthraquinones in Cassiae Semen. Two conventional adsorbents, C₁₈ and silica gel were investigated. The strategy included two steps: Extraction and determination. Wasted crab shells were used as an alternative adsorbent and ionic liquid was used as an alternative solvent in the first step. Factors affecting extraction efficiency were optimized: A sample/adsorbent ratio of 2:1, a grinding time of 3 min, a vortex time of 3 min, and ionic liquid ([Domim]HSO₄, 250 mM) was used as eluent in the VS-MSPD procedure. As a result, the established method provided satisfactory linearity (R > 0.999), good accuracy and high reproducibility (RSD < 4.60%), and it exhibited the advantages of smaller sample amounts, shorter extraction time, less volume of elution solvent, and was much more environmental-friendly when compared with other conventional methods. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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12 pages, 1489 KiB

Open AccessArticle

A Vortex-Assisted Dispersive Liquid-Liquid Microextraction Followed by UPLC-MS/MS for Simultaneous Determination of Pesticides and Aflatoxins in Herbal Tea

by Rui Zhang, Zhen-Chao Tan, Ke-Cheng Huang, Yan Wen, Xiang-Ying Li, Jun-Long Zhao and Cheng-Lan Liu

Molecules 2019, 24(6), 1029; https://doi.org/10.3390/molecules24061029 - 15 Mar 2019

Cited by 31 | Viewed by 3783

Abstract

A method for detecting the organophosphorus pesticides residue and aflatoxins in China herbal tea has been developed by UPLC-MS/MS coupled with vortex-assisted dispersive liquid-liquid microextraction (DLLME). The extraction conditions for vortex-assisted DLLME extraction were optimized using single-factor experiments and response surface design. The [...] Read more.

A method for detecting the organophosphorus pesticides residue and aflatoxins in China herbal tea has been developed by UPLC-MS/MS coupled with vortex-assisted dispersive liquid-liquid microextraction (DLLME). The extraction conditions for vortex-assisted DLLME extraction were optimized using single-factor experiments and response surface design. The optimum conditions for the experiment were the pH 5.1, 347 µL of chloroform (extraction solvent) and 1614 µL of acetonitrile (dispersive solvent). Under the optimum conditions, the targets were good linearity in the range of 0.1 µg/L–25 µg/L and the correlation coefficient above 0.9998. The mean recoveries of all analytes were in the ranged from 70.06%–115.65% with RSDs below 8.54%. The detection limits were in the range of 0.001 µg/L–0.01µg/L. The proposed method is a fast and effective sample preparation with good enrichment and extraction efficiency, which can simultaneously detect pesticides and aflatoxins in China herbal tea. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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10 pages, 2175 KiB

Open AccessArticle

Multi-Spheres Adsorptive Microextraction (MSAμE)—Application of a Novel Analytical Approach for Monitoring Chemical Anthropogenic Markers in Environmental Water Matrices

by Ana R. M. Silva, Nuno R. Neng and José M. F. Nogueira

Molecules 2019, 24(5), 931; https://doi.org/10.3390/molecules24050931 - 7 Mar 2019

Cited by 3 | Viewed by 2518

Abstract

Multi-spheres adsorptive microextraction using powdered activated carbons (ACs) was studied as a novel enrichment approach, followed by liquid desorption and high-performance liquid chromatography with diode array detection (MSAµE(AC)-LD/HPLC-DAD) to monitor caffeine (CAF) and acetaminophen (ACF) traces in environmental matrices. In this study, commercial [...] Read more.

Multi-spheres adsorptive microextraction using powdered activated carbons (ACs) was studied as a novel enrichment approach, followed by liquid desorption and high-performance liquid chromatography with diode array detection (MSAµE(AC)-LD/HPLC-DAD) to monitor caffeine (CAF) and acetaminophen (ACF) traces in environmental matrices. In this study, commercial activated carbons (N, N_OX, and R) were tested, with the latter showing a much better performance for the analysis of both anthropogenic drugs. The main parameters affecting the efficiency of the proposed methodology are fully discussed using commercial AC(R). Textural and surface chemistry properties of the ACs sample were correlated with the analytical results. Assays performed on 30 mL of water samples spiked at 10 µg L⁻¹ under optimized experimental conditions, yielding recoveries of 75.3% for ACF and 82.6% for CAF. The methodology also showed excellent linear dynamic ranges for both drugs with determination coefficients higher than 0.9976, limits of detection and quantification of 0.8–1.2 µg L⁻¹ and 2.8–4.0 µg L⁻¹, respectively, and suitable precision (RSD < 13.8%). By using the standard addition method, the application of the present method to environmental matrices, including superficial, sea, and wastewater samples, allowed very good performance at the trace level. The proposed methodology proved to be a feasible alternative for polar compound analysis, showing to be easy to implement, reliable, and sensitive, with the possibility to reuse and store the analytical devices loaded with the target compounds for later analysis. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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11 pages, 4336 KiB

Open AccessArticle

Comparison of the Partition Efficiencies of Multiple Phenolic Compounds Contained in Propolis in Different Modes of Acetonitrile–Water-Based Homogenous Liquid–Liquid Extraction

by Wenbin Chen, Xijuan Tu, Dehui Wu, Zhaosheng Gao, Siyuan Wu and Shaokang Huang

Molecules 2019, 24(3), 442; https://doi.org/10.3390/molecules24030442 - 26 Jan 2019

Cited by 20 | Viewed by 4876

Abstract

Homogeneous liquid–liquid extraction (HLLE) has attracted considerable interest in the sample preparation of multi-analyte analysis. In this study, HLLEs of multiple phenolic compounds in propolis, a polyphenol-enriched resinous substance collected by honeybees, were performed for improving the understanding of the differences in partition [...] Read more.

Homogeneous liquid–liquid extraction (HLLE) has attracted considerable interest in the sample preparation of multi-analyte analysis. In this study, HLLEs of multiple phenolic compounds in propolis, a polyphenol-enriched resinous substance collected by honeybees, were performed for improving the understanding of the differences in partition efficiencies in four acetonitrile–water-based HLLE methods, including salting-out assisted liquid–liquid extraction (SALLE), sugaring-out assisted liquid–liquid extraction (SULLE), hydrophobic-solvent assisted liquid–liquid extraction (HSLLE), and subzero-temperature assisted liquid–liquid extraction (STLLE). Phenolic compounds were separated in reversed-phase HPLC, and the partition efficiencies in different experimental conditions were evaluated. Results showed that less-polar phenolic compounds (kaempferol and caffeic acid phenethyl ester) were highly efficiently partitioned into the upper acetonitrile (ACN) phase in all four HLLE methods. For more-polar phenolic compounds (caffeic acid, p-coumaric acid, isoferulic acid, dimethoxycinnamic acid, and cinnamic acid), increasing the concentration of ACN in the ACN–H₂O mixture could dramatically improve the partition efficiency. Moreover, results indicated that NaCl-based SALLE, HSLLE, and STLLE with ACN concentrations of 50:50 (ACN:H₂O, v/v) could be used for the selective extraction of low-polarity phenolic compounds. MgSO₄-based SALLE in the 50:50 ACN–H₂O mixture (ACN:H₂O, v/v) and the NaCl-based SALLE, SULLE, and STLLE with ACN concentrations of 70:30 (ACN:H₂O, v/v) could be used as general extraction methods for multiple phenolic compounds. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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13 pages, 2621 KiB

Open AccessArticle

Butyl Methacrylate-Co-Ethylene Glycol Dimethacrylate Monolith for Online in-Tube SPME-UHPLC-MS/MS to Determine Chlopromazine, Clozapine, Quetiapine, Olanzapine, and Their Metabolites in Plasma Samples

by Luiz G. M. Beloti, Luis F. C. Miranda and Maria Eugênia C. Queiroz

Molecules 2019, 24(2), 310; https://doi.org/10.3390/molecules24020310 - 16 Jan 2019

Cited by 21 | Viewed by 4973

Abstract

This manuscript describes a sensitive, selective, and online in-tube solid-phase microextraction coupled with an ultrahigh performance liquid chromatography-tandem mass spectrometry (in-tube SPME-UHPLC-MS/MS) method to determine chlopromazine, clozapine, quetiapine, olanzapine, and their metabolites in plasma samples from schizophrenic patients. Organic poly(butyl methacrylate-co-ethylene glycol dimethacrylate) [...] Read more.

This manuscript describes a sensitive, selective, and online in-tube solid-phase microextraction coupled with an ultrahigh performance liquid chromatography-tandem mass spectrometry (in-tube SPME-UHPLC-MS/MS) method to determine chlopromazine, clozapine, quetiapine, olanzapine, and their metabolites in plasma samples from schizophrenic patients. Organic poly(butyl methacrylate-co-ethylene glycol dimethacrylate) monolith was synthesized on the internal surface of a fused silica capillary (covalent bonds) for in-tube SPME. Analyte extraction and analysis was conducted by connecting the monolithic capillary to an UHPLC-MS/MS system. The monolith was characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectrometry (FTIR). The developed method presented adequate linearity for all the target antipsychotics: R² was higher than 0.9975, lack-of-fit ranged from 0.115 to 0.955, precision had variation coefficients lower than 14.2%, and accuracy had relative standard error values ranging from −13.5% to 14.6%, with the exception of the lower limit of quantification (LLOQ). The LLOQ values in plasma samples were 10 ng mL⁻¹ for all analytes. The developed method was successfully applied to determine antipsychotics and their metabolites in plasma samples from schizophrenic patients. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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13 pages, 3913 KiB

Open AccessArticle

Evaluation of Polyvinyl Alcohol/Pectin-Based Hydrogel Disks as Extraction Phase for Determination of Steroidal Hormones in Aqueous Samples by GC-MS/MS

by Naiara M. F. M. Sampaio, Natara D. B. Castilhos, Bruno C. da Silva, Izabel C. Riegel-Vidotti and Bruno J. G. Silva

Molecules 2019, 24(1), 40; https://doi.org/10.3390/molecules24010040 - 22 Dec 2018

Cited by 20 | Viewed by 3874

Abstract

A new extraction phase based on hydrogel disks of polyvinyl alcohol (PVOH) and pectin was proposed, characterized and evaluated for the extraction of six steroidal hormones (estriol, estrone, 17β-estradiol, 17α-ethinylestradiol, progesterone, and testosterone) in aqueous samples with subsequent determination by gas chromatography-tandem mass [...] Read more.

A new extraction phase based on hydrogel disks of polyvinyl alcohol (PVOH) and pectin was proposed, characterized and evaluated for the extraction of six steroidal hormones (estriol, estrone, 17β-estradiol, 17α-ethinylestradiol, progesterone, and testosterone) in aqueous samples with subsequent determination by gas chromatography-tandem mass spectrometry (GC-MS/MS) after the derivatization procedure. The developed extraction procedure was based on the solid phase extraction (SPE) technique, but employed hydrogel as the sorbent phase. The effects of several parameters, including the amount and composition of the sorbent phase, pH, sample volume, flow rate, and gel swelling over the extraction efficiency, were evaluated. Gels with lower swelling indexes and larger amounts of sorbent ensured higher extraction yields of analytes. The main benefits of using the PVOH/pectin-based hydrogel as the extraction phase are the ease of synthesis, low-cost preparation, and the possibility of reusing the extraction disks. Limits of quantification of 0.5 μg L⁻¹ for estrone and 17β-estradiol, and 1 μg L⁻¹ for testosterone, 17α-ethinylestradiol, progesterone, and estriol were obtained. Accuracy values ranged from 80% to 110%, while the inter-assay precision ranged from 0.23% to 22.2% and the intra-assay from 0.55% to 12.3%. Since the sorbent phase has an amphiphilic character, the use of hydrogels is promising for the extraction of medium-to-high polarity compounds. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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11 pages, 4381 KiB

Open AccessArticle

High-Frequency Heating Extraction Method for Sensitive Drug Analysis in Human Nails

by Fumiki Takahashi, Masaru Kobayashi, Atsushi Kobayashi, Kanya Kobayashi and Hideki Asamura

Molecules 2018, 23(12), 3231; https://doi.org/10.3390/molecules23123231 - 7 Dec 2018

Cited by 9 | Viewed by 3418

Abstract

Background: A simple, sensitive, and rapid extraction method based on high-frequency (H-F) heating was developed for drug analysis in human nails. Methods: A human nail was placed in a glass tube with an extraction solvent (methanol and 0.1% formic acid; 7:3, v/ [...] Read more.

Background: A simple, sensitive, and rapid extraction method based on high-frequency (H-F) heating was developed for drug analysis in human nails. Methods: A human nail was placed in a glass tube with an extraction solvent (methanol and 0.1% formic acid; 7:3, v/v), and a ferromagnetic alloy (pyrofoil) was wrapped in a spiral around the glass tube. Then, the glass tube was placed in a Curie point pyrolyzer, and a H-F alternating voltage (600 kHz) was applied. The sample and extraction solvent were heated at the Curie temperature for 3 min. Different Curie temperatures were applied by changing the pyrofoil (160 °C, 170 °C, 220 °C, and 255 °C). Results: The caffeine in the nail was effectively and rapidly extracted into the extraction solvent with the pyrofoil at 220 °C. The peak area obtained for the caffeine using liquid chromatography mass spectrometry (LC-MS/MS) was five times that of what was obtained after conventional ultrasonic irradiation extraction. Because the extraction uses high-pressure and high-temperature conditions in a test tube, the drugs that were strongly incorporated in nails could be extracted into the solvent. The amount of caffeine extracted was independent of the size of the pieces in the sample. Conclusions: Therefore, the sensitive determination of target drugs in nails is possible with rapid (20 min, including H-F extraction for 3 min) and simple sample preparation. The developed method was applied to a nail from a patient with hypertension. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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14 pages, 1001 KiB

Open AccessArticle

Optimization of Vortex-Assisted Dispersive Liquid-Liquid Microextraction for the Simultaneous Quantitation of Eleven Non-Anthocyanin Polyphenols in Commercial Blueberry Using the Multi-Objective Response Surface Methodology and Desirability Function Approach

by Ying Xue, Xian-Shun Xu, Li Yong, Bin Hu, Xing-De Li, Shi-Hong Zhong, Yi Li, Jing Xie and Lin-Sen Qing

Molecules 2018, 23(11), 2921; https://doi.org/10.3390/molecules23112921 - 9 Nov 2018

Cited by 6 | Viewed by 3209

Abstract

In the present study, 11 non-anthocyanin polyphenols, gallic acid, protocatechuate, vanillic acid, syringic acid, ferulic acid, quercetin, catechin, epicatechin, epigallocatechin gallate, gallocatechin gallate and epicatechin gallate—were firstly screened and identified from blueberries using an ultra performance liquid chromatography–time of flight mass spectrography (UPLC-TOF/MS) [...] Read more.

In the present study, 11 non-anthocyanin polyphenols, gallic acid, protocatechuate, vanillic acid, syringic acid, ferulic acid, quercetin, catechin, epicatechin, epigallocatechin gallate, gallocatechin gallate and epicatechin gallate—were firstly screened and identified from blueberries using an ultra performance liquid chromatography–time of flight mass spectrography (UPLC-TOF/MS) method. Then, a sample preparation method was developed based on vortex-assisted dispersive liquid-liquid microextraction. The microextraction conditions, including the amount of ethyl acetate, the amount of acetonitrile and the solution pH, were optimized through the multi-objective response surface methodology and desirability function approach. Finally, an ultra performance liquid chromatography–triple quadrupole mass spectrography (UPLC-QqQ/MS) method was developed to determine the 11 non-anthocyanin polyphenols in 25 commercial blueberry samples from Sichuan province and Chongqing city. The results show that this new method with high accuracy, good precision and simple operation characteristics, can be used to determine non-anthocyanin polyphenols in blueberries and is expected to be used in the analysis of other fruits and vegetables. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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Review

Jump to: Research

20 pages, 1651 KiB

Open AccessReview

Sample Digestion and Combined Preconcentration Methods for the Determination of Ultra-Low Gold Levels in Rocks

by Yan-hong Liu, Bo Wan and Ding-shuai Xue

Molecules 2019, 24(9), 1778; https://doi.org/10.3390/molecules24091778 - 8 May 2019

Cited by 14 | Viewed by 4798

Abstract

The gold abundance in basic rocks, which normally varies between 0.5 and 5 ppb, has served as a very important indicator in many geoscience studies, including those focused on the planetary differentiation, redistribution of elements during the crustal process, and ore genesis. However, [...] Read more.

The gold abundance in basic rocks, which normally varies between 0.5 and 5 ppb, has served as a very important indicator in many geoscience studies, including those focused on the planetary differentiation, redistribution of elements during the crustal process, and ore genesis. However, because gold is a monoisotopic element that exhibits a nugget effect, it is very difficult to quantify its ultra-low levels in rocks, which significantly limits our understanding of the origin of gold and its circulation between the Earth crust, mantle, and core. In this work, we summarize various sample digestion and combined preconcentration methods for the determination of gold amounts in rocks. They include fire assay, fire assay combined with Te coprecipitation and instrumental neutron activation analysis (INAA) or laser ablation inductively coupled plasma mass spectrometry, fusion combined with Te coprecipitation and anion exchange resins, dry chlorination, wet acid digestion combined with precipitation, ion exchange resins, solvent extraction, polyurethane foam, extraction chromatography, novel solid adsorbents, and direct determination by INAA. In addition, the faced challenges and future perspectives in this field are discussed. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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38 pages, 4100 KiB

Open AccessReview

Modern Methods of Sample Preparation for the Analysis of Oxylipins in Biological Samples

by Ivan Liakh, Alicja Pakiet, Tomasz Sledzinski and Adriana Mika

Molecules 2019, 24(8), 1639; https://doi.org/10.3390/molecules24081639 - 25 Apr 2019

Cited by 43 | Viewed by 8909

Abstract

Oxylipins are potent lipid mediators derived from polyunsaturated fatty acids, which play important roles in various biological processes. Being important regulators and/or markers of a wide range of normal and pathological processes, oxylipins are becoming a popular subject of research; however, the low [...] Read more.

Oxylipins are potent lipid mediators derived from polyunsaturated fatty acids, which play important roles in various biological processes. Being important regulators and/or markers of a wide range of normal and pathological processes, oxylipins are becoming a popular subject of research; however, the low stability and often very low concentration of oxylipins in samples are a significant challenge for authors and continuous improvement is required in both the extraction and analysis techniques. In recent years, the study of oxylipins has been directly related to the development of new technological platforms based on mass spectrometry (LC–MS/MS and gas chromatography–mass spectrometry (GC–MS)/MS), as well as the improvement in methods for the extraction of oxylipins from biological samples. In this review, we systematize and compare information on sample preparation procedures, including solid-phase extraction, liquid–liquid extraction from different biological tissues. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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13 pages, 372 KiB

Open AccessReview

A Review on the Recent Progress in Matrix Solid Phase Dispersion

by Xijuan Tu and Wenbin Chen

Molecules 2018, 23(11), 2767; https://doi.org/10.3390/molecules23112767 - 25 Oct 2018

Cited by 57 | Viewed by 6556

Abstract

Matrix solid phase dispersion (MSPD) has proven to be an efficient sample preparation method for solid, semi-solid, and viscous samples. Applications of MSPD have covered biological, food, and environmental samples, including both organic and inorganic analytes. This review presents an update on the [...] Read more.

Matrix solid phase dispersion (MSPD) has proven to be an efficient sample preparation method for solid, semi-solid, and viscous samples. Applications of MSPD have covered biological, food, and environmental samples, including both organic and inorganic analytes. This review presents an update on the development of MSPD in the period 2015~June 2018. In the first part of this review, we focus on the latest development in MSPD sorbent, including molecularly imprinted polymers, and carbon-based nanomaterials etc. The second part presents the miniaturization of MSPD, discussing the progress in both micro-MSPD and mini-MSPD. The on-line/in-line techniques for improving the automation and sample throughput are also discussed. The final part summarizes the success in the modification of original MSPD procedures. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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25 pages, 496 KiB

Open AccessReview

A Review of the Extraction and Determination Methods of Thirteen Essential Vitamins to the Human Body: An Update from 2010

by Yuan Zhang, Wei-e Zhou, Jia-qing Yan, Min Liu, Yu Zhou, Xin Shen, Ying-lin Ma, Xue-song Feng, Jun Yang and Guo-hui Li

Molecules 2018, 23(6), 1484; https://doi.org/10.3390/molecules23061484 - 19 Jun 2018

Cited by 130 | Viewed by 13704

Abstract

Vitamins are a class of essential nutrients in the body; thus, they play important roles in human health. The chemicals are involved in many physiological functions and both their lack and excess can put health at risk. Therefore, the establishment of methods for [...] Read more.

Vitamins are a class of essential nutrients in the body; thus, they play important roles in human health. The chemicals are involved in many physiological functions and both their lack and excess can put health at risk. Therefore, the establishment of methods for monitoring vitamin concentrations in different matrices is necessary. In this review, an updated overview of the main pretreatments and determination methods that have been used since 2010 is given. Ultrasonic assisted extraction, liquid–liquid extraction, solid phase extraction and dispersive liquid–liquid microextraction are the most common pretreatment methods, while the determination methods involve chromatography methods, electrophoretic methods, microbiological assays, immunoassays, biosensors and several other methods. Different pretreatments and determination methods are discussed. Full article

(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)

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