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Solid-Phase Microextraction and Related Techniques in Bioanalysis
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Solid-Phase Microextraction and Related Techniques in Bioanalysis

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

Deadline for manuscript submissions: closed (30 April 2022) | Viewed by 32091

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

Special Issue Editor

Prof. Dr. Hiroyuki Kataoka

E-Mail Website
Guest Editor
School of Pharmacy, Shujitsu University, 1-6-1, Nishigawara, Okayama 703-8516, Japan
Interests: solid-phase microextraction; chromatography; advanced glycation end products; stress hormone; biomarker; heterocyclic amines; polycyclic aromatic hydrocarbons; LC–MS/MS analysis
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Bioanalysis of endogenous substances, drugs and their metabolites, disease biomarkers, contaminants, poisons, etc. is important in biological function analysis, metabolomics, new drug development, therapeutic drug monitoring, doping control, forensic toxicology, patient diagnosis and the biomonitoring of human exposure to hazardous chemicals. In these analyses, sample preparation is essential for the isolation and concentration of target analytes from complex biological matrices, such as serum/plasma, urine, saliva, hair, nail, sweat, exhaled breath, and tissue. However, this process is time-consuming, labor-intensive and error-prone, and markedly influences the reliability and accuracy of determining molecules of interest. Thus, efficient sample preparation techniques and their integration with various analytical instruments have become a significant challenge.

Solid-phase microextraction (SPME) is a simple and convenient sample preparation technique that has enabled automation, miniaturization, high-throughput performance, and online coupling with analytical instruments. Moreover, SPME has reduced analysis times, as well as the costs of solvents and disposal. Since SPME was first introduced in the early 1990s by Arthur and Pawliszyn, more robust fiber assemblies and coatings with higher extraction efficiencies, selectivity and stability have been commercialized. Furthermore, new geometries have been designed to use capillary tubes, magnetic stir bars or thin films for extraction devices rather than fibers, and novel intelligent polymer coatings with great sorption capacity or good selectivity have been developed as extraction phases.

This Special Issue will include a wide range of topics covering not only the development of SPME and related techniques and their applications for bioanalysis, but also the development of new extraction devices and novel intelligent coating materials available for bioanalytical, biomimetic and biocompatible sample preparation. I hope that scientists will find the selected up-to-date topics regarding sample preparation of interest, and that additional ideas and new technologies may emerge from this Special Issue.

Prof. Dr. Hiroyuki Kataoka
Guest Editor

Manuscript Submission Information

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Keywords

  • solid phase microextraction
  • in-tube solid phase microextraction
  • stir bar sorptive extraction
  • thin-film microextraction
  • microextraction in packed syringe
  • solid phase dynamic extraction
  • in-tip microextraction
  • immunosorbents
  • restricted access materials
  • molecularly imprinted polymers
  • porous organic frameworks
  • ionic liquids
  • sol–gel-based sorbents
  • carbon-based sorbents
  • magnetic nanoparticles
  • monolithic polymers
  • in vivo sampling
  • biomedical analysis
  • pharmaceutical analysis
  • forensic analysis

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Editorial

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4 pages, 211 KiB  
Editorial
Solid-Phase Microextraction and Related Techniques in Bioanalysis
by Hiroyuki Kataoka
Molecules 2023, 28(6), 2467; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28062467 - 08 Mar 2023
Cited by 1 | Viewed by 983
Abstract
Living organisms, such as microorganisms, plants and animals, are composed of complex constituents, which may include bioactive components that maintain their functions [...] Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)

Research

Jump to: Editorial

13 pages, 3789 KiB  
Article
In Vitro and In Vivo Human Body Odor Analysis Method Using GO:PANI/ZNRs/ZIF−8 Adsorbent Followed by GC/MS
by Sehyun Kim and Sunyoung Bae
Molecules 2022, 27(15), 4795; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27154795 - 27 Jul 2022
Cited by 6 | Viewed by 1675
Abstract
Among various volatile organic compounds (VOCs) emitted from human skin, trans-2-nonenal, benzothiazole, hexyl salicylate, α-hexyl cinnamaldehyde, and isopropyl palmitate are key indicators associated with the degrees of aging. In our study, extraction and determination methods of human body odor are newly developed [...] Read more.
Among various volatile organic compounds (VOCs) emitted from human skin, trans-2-nonenal, benzothiazole, hexyl salicylate, α-hexyl cinnamaldehyde, and isopropyl palmitate are key indicators associated with the degrees of aging. In our study, extraction and determination methods of human body odor are newly developed using headspace-in needle microextraction (HS-INME). The adsorbent was synthesized with graphene oxide:polyaniline/zinc nanorods/zeolitic imidazolate framework-8 (GO:PANI/ZNRs/ZIF−8). Then, a wire coated with the adsorbent was placed into the adsorption kit to be directly exposed to human skin as in vivo sampling and inserted into the needle so that it was able to be desorbed at the GC injector. The adsorption kit was made in-house with a 3D printer. For the in vitro method, the wire coated with the adsorbent was inserted into the needle and exposed to the headspace of the vial. When a cotton T-shirt containing body odor was transferred to a vial, the headspace of the vial was saturated with body odor VOCs. After volatile organic compounds were adsorbed in the dynamic mode, the needle was transferred to the injector for analysis of the volatile organic compounds by gas chromatography/mass spectrometry (GC/MS). The conditions of adsorbent fabrication and extraction for body odor compounds were optimized by response surface methodology (RSM). In conclusion, it was able to synthesize GO:PANI/ZNRs/ZIF−8 at the optimal condition and applicable to both in vivo and in vitro methods for body odor VOCs analysis. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)
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12 pages, 1872 KiB  
Article
Online In-Tube Solid-Phase Microextraction Coupled with Liquid Chromatography–Tandem Mass Spectrometry for Automated Analysis of Four Sulfated Steroid Metabolites in Saliva Samples
by Hiroyuki Kataoka and Daiki Nakayama
Molecules 2022, 27(10), 3225; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27103225 - 18 May 2022
Cited by 9 | Viewed by 1581
Abstract
Accurate measurement of sulfated steroid metabolite concentrations can not only enable the elucidation of the mechanisms regulating steroid metabolism, but also lead to the diagnosis of various related diseases. The present study describes a simple and sensitive method for the simultaneous determination of [...] Read more.
Accurate measurement of sulfated steroid metabolite concentrations can not only enable the elucidation of the mechanisms regulating steroid metabolism, but also lead to the diagnosis of various related diseases. The present study describes a simple and sensitive method for the simultaneous determination of four sulfated steroid metabolites in saliva, pregnenolone sulfate (PREGS), dehydroepiandrosterone sulfate (DHEAS), cortisol sulfate (CRTS), and 17β-estradiol-3-sulfate (E2S), by online coupling of in-tube solid-phase microextraction (IT-SPME) and stable isotope dilution liquid chromatography–tandem mass spectrometry (LC–MS/MS). These compounds were extracted and concentrated on Supel-Q PLOT capillary tubes by IT-SPME and separated and detected within 6 min by LC–MS/MS using an InertSustain swift C18 column and negative ion mode multiple reaction monitoring systems. These operations were fully automated by an online program. Calibration curves using their stable isotope-labeled internal standards showed good linearity in the range of 0.01–2 ng mL−1 for PREGS, DHEAS, and CRTS and of 0.05–10 ng mL−1 for E2S. The limits of detection (S/N = 3) of PREGS, DHEAS, CRTS, and E2S were 0.59, 0.30, 0.80, and 3.20 pg mL−1, respectively. Moreover, intraday and interday variations were lower than 11.1% (n = 5). The recoveries of these compounds from saliva samples were in the range of 86.6–112.9%. The developed method is highly sensitive and specific and can easily measure sulfated steroid metabolite concentrations in 50 μL saliva samples. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)
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14 pages, 4447 KiB  
Article
Smart Titanium Wire Used for the Evaluation of Hydrophobic/Hydrophilic Interaction by In-Tube Solid Phase Microextraction
by Yuping Zhang, Ning Wang, Zhenyu Lu, Na Chen, Chengxing Cui and Xinxin Chen
Molecules 2022, 27(7), 2353; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27072353 - 06 Apr 2022
Cited by 8 | Viewed by 1611
Abstract
Evaluation of the hydrophobic/hydrophilic interaction individually between the sorbent and target compounds in sample pretreatment is a big challenge. Herein, a smart titanium substrate with switchable surface wettability was fabricated and selected as the sorbent for the solution. The titanium wires and meshes [...] Read more.
Evaluation of the hydrophobic/hydrophilic interaction individually between the sorbent and target compounds in sample pretreatment is a big challenge. Herein, a smart titanium substrate with switchable surface wettability was fabricated and selected as the sorbent for the solution. The titanium wires and meshes were fabricated by simple hydrothermal etching and chemical modification so as to construct the superhydrophilic and superhydrophobic surfaces. The micro/nano hierarchical structures of the formed TiO2 nanoparticles in situ on the surface of Ti substrates exhibited the switchable surface wettability. After UV irradiation for about 15.5 h, the superhydrophobic substrates became superhydrophilic. The morphologies and element composition of the wires were observed by SEM, EDS, and XRD, and their surface wettabilities were measured using the Ti mesh by contact angle goniometer. The pristine hydrophilic wire, the resulting superhydrophilic wire, superhydrophobic wire, and the UV-irradiated superhydrophilic wire were filled into a stainless tube as the sorbent instead of the sample loop of a six-port valve for on-line in-tube solid-phase microextraction. When employed in conjunction with HPLC, four kinds of wires were comparatively applied to extract six estrogens in water samples. The optimal conditions for the preconcentration and separation of target compounds were obtained with a sample volume of 60 mL, an injection rate of 2 mL/min, a desorption time of 2 min, and a mobile phase of acetonile/water (47/53, v/v). The results showed that both the superhydrophilic wire and UV-irradiated wire had the highest extraction efficiency for the polar compounds of estrogens with the enrichment factors in the range of 20–177, while the superhydrophobic wire exhibited the highest extraction efficiency for the non-polar compounds of five polycyclic aromatic hydrocarbons (PAHs). They demonstrated that extraction efficiency was mainly dependent on the surface wettability of the sorbent and the polarity of the target compounds, which was in accordance with the molecular theory of like dissolves like. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)
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10 pages, 975 KiB  
Article
Identification of Biomarker Volatile Organic Compounds Released by Three Stored-Grain Insect Pests in Wheat
by Lijun Cai, Sarina Macfadyen, Baozhen Hua, Haochuan Zhang, Wei Xu and Yonglin Ren
Molecules 2022, 27(6), 1963; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27061963 - 17 Mar 2022
Cited by 8 | Viewed by 2077
Abstract
Monitoring and early detection of stored-grain insect infestation is essential to implement timely and effective pest management decisions to protect stored grains. We report a reliable analytical procedure based on headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry (HS-SPME-GC-MS) to assess stored-grain infestation [...] Read more.
Monitoring and early detection of stored-grain insect infestation is essential to implement timely and effective pest management decisions to protect stored grains. We report a reliable analytical procedure based on headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry (HS-SPME-GC-MS) to assess stored-grain infestation through the detection of volatile compounds emitted by insects. Four different fibre coatings were assessed; 85 µm CAR/PDMS had optimal efficiency in the extraction of analytes from wheat. The headspace profiles of volatile compounds produced by Tribolium castaneum (Herbst), Rhyzopertha dominica (Fabricius), and Sitophilus granarius (Linnaeus), either alone or with wheat, were compared with those of non-infested wheat grains. Qualitative analysis of chromatograms showed the presence of different volatile compound profiles in wheat with pest infestation compared with the wheat controls. Wheat-specific and insect-specific volatile compounds were identified, including the aggregation pheromones, dominicalure-1 and dominicalure-2, from R. dominica, and benzoquinones homologs from T. castaneum. For the first time, the presence of 3-hydroxy-2-butanone was reported from S. granarius, which might function as an alarm pheromone. These identified candidate biomarker compounds can be utilized in insect surveillance and monitoring in stored grain to safeguard our grain products in future. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)
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19 pages, 43097 KiB  
Article
Profile of Myracrodruon urundeuva Volatile Compounds Ease of Extraction and Biodegradability and In Silico Evaluation of Their Interactions with COX-1 and iNOS
by Yuri G. Figueiredo, Eduardo A. Corrêa, Afonso H. de Oliveira Junior, Ana C. d. C. Mazzinghy, Henrique d. O. P. Mendonça, Yan J. G. Lobo, Yesenia M. García, Marcelo A. d. S. Gouvêia, Ana C. C. F. F. de Paula, Rodinei Augusti, Luisa D. C. B. Reina, Carlos H. da Silveira, Leonardo H. F. de Lima and Júlio O. F. Melo
Molecules 2022, 27(5), 1633; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27051633 - 01 Mar 2022
Cited by 3 | Viewed by 2168
Abstract
Myracrodruon urundeuva Fr. Allem. (Anacardiaceae) is a tree popularly known as the “aroeira-do-sertão”, native to the caatinga and cerrado biomes, with a natural dispersion ranging from the Northeast, Midwest, to Southeast Brazil. Its wood is highly valued and overexploited, due to its characteristics [...] Read more.
Myracrodruon urundeuva Fr. Allem. (Anacardiaceae) is a tree popularly known as the “aroeira-do-sertão”, native to the caatinga and cerrado biomes, with a natural dispersion ranging from the Northeast, Midwest, to Southeast Brazil. Its wood is highly valued and overexploited, due to its characteristics such as durability and resistance to decaying. The diversity of chemical constituents in aroeira seed has shown biological properties against microorganisms and helminths. As such, this work aimed to identify the profile of volatile compounds present in aroeira seeds. Headspace solid phase microextraction was employed (HS-SPME) using semi-polar polydimethylsiloxane-divinylbenzene fiber (PDMS/DVB) for the extraction of VOCs. 22 volatile organic compounds were identified: nine monoterpenes and eight sesquiterpenes, in addition to six compounds belonging to different chemical classes such as fatty acids, terpenoids, salicylates and others. Those that stood out were p-mentha-1,4, 4(8)-diene, 3-carene (found in all samples), caryophyllene and cis-geranylacetone. A virtual docking analysis suggested that around 65% of the VOCs molar content from the aroeiras seeds present moderate a strong ability to bind to cyclooxygenase I (COX-I) active site, oxide nitric synthase (iNOS) active site (iNOSas) or to iNOS cofactor site (iNOScs), corroborating an anti-inflamatory potential. A pharmacophoric descriptor analysis allowed to infer the more determinant characteristics of these compounds’ conferring affinity to each site. Taken together, our results illustrate the high applicability for the integrated use of SPME, in silico virtual screening and chemoinformatics tools at the profiling of the biotechnological and pharmaceutical potential of natural sources. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)
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13 pages, 1173 KiB  
Article
Response of Aphid Parasitoids to Volatile Organic Compounds from Undamaged and Infested Brassica oleracea with Myzus persicae
by Qasim Ahmed, Manjree Agarwal, Ruaa Alobaidi, Haochuan Zhang and Yonglin Ren
Molecules 2022, 27(5), 1522; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27051522 - 24 Feb 2022
Cited by 9 | Viewed by 2644
Abstract
Headspace solid microextraction (HS-SPME) and GC-MS were used to investigate volatile organic compounds (VOCs) from cabbage plants infested and uninfested with green peach aphid Myzus persicae. The HS-SPME combined with GC-MS analysis of the volatiles described the differences between the infested and [...] Read more.
Headspace solid microextraction (HS-SPME) and GC-MS were used to investigate volatile organic compounds (VOCs) from cabbage plants infested and uninfested with green peach aphid Myzus persicae. The HS-SPME combined with GC-MS analysis of the volatiles described the differences between the infested and uninfested cabbage. Overall, 28 compounds were detected in infested and uninfested cabbage. Some VOCs released from infested cabbage were greater than uninfested plants and increased the quantity of the composition from infested plants. According to the peak area from the GC-MS analysis, the VOCs from infested cabbage consisted of propane, 2-methoxy, alpha- and beta pinene, myrcene, 1-hexanone, 5-methyl-1-phenyl-, limonene, decane, gamma-terpinen and heptane, 2,4,4-trimethyl. All these volatiles were higher in the infested cabbage compared with their peak area in the uninfested cabbage. The results of the study using a Y-shape olfactometer revealed that the VOCs produced by infested cabbage attracted Myzus persicae substantially more than uninfested plants or clean air. The percentage of aphid choice was 80% in favor of infested cabbage; 7% were attracted to the clean air choice and uninfested plants. A total of aphids 7% were attracted to clean air. Comparing between infested and uninfested cabbage plants, the aphid was attracted to 63% of the infested cabbage, versus 57% of the uninfested cabbage. The preferences of Aphidus colemani and Aphelinus abdominalis to the infested or uninfested plants with M. persicae and compared with clean air indicated that parasitoids could discriminate the infested cabbage. Both parasitoids significantly responded to the plant odor and were attracted to 86.6% of the infested cabbage plants. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)
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12 pages, 2186 KiB  
Article
The Difference of Volatile Compounds in Female and Male Buds of Herpetospermum pedunculosum Based on HS-SPME-GC-MS and Multivariate Statistical Analysis
by Zhenying Liu, Ye Fang, Cui Wu, Xian Hai, Bo Xu, Zhuojun Li, Pingping Song, Huijun Wang and Zhimao Chao
Molecules 2022, 27(4), 1288; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27041288 - 14 Feb 2022
Cited by 6 | Viewed by 1456
Abstract
Herpetospermum pedunculosum (Ser.) C. B. Clarke (Family Cucurbitaceae) is a dioecious plant and has been used as a traditional Tibetan medicine for the treatment of hepatobiliary diseases. The component, content, and difference in volatile compounds in the female and male buds of H [...] Read more.
Herpetospermum pedunculosum (Ser.) C. B. Clarke (Family Cucurbitaceae) is a dioecious plant and has been used as a traditional Tibetan medicine for the treatment of hepatobiliary diseases. The component, content, and difference in volatile compounds in the female and male buds of H. pedunculosum were explored by using headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) technology and multivariate statistical analysis. The results showed that isoamyl alcohol was the main compound in both female and male buds and its content in males was higher than that in females; 18 compounds were identified in female buds including 6 unique compounds such as (E)-4-hexenol and isoamyl acetate, and 32 compounds were identified in male buds, including 20 unique compounds such as (Z)-3-methylbutyraldehyde oxime and benzyl alcohol. (Z)-3-methylbutyraldehyde oxime and (E)-3-methylbutyraldehyde oxime were found in male buds, which only occurred in night-flowering plants. In total, 9 differential volatile compounds between female and male buds were screened out, including isoamyl alcohol, (Z)-3-methylbutanal oxime, and 1-nitropentane based on multivariate statistical analysis such as principal component analysis (PCA) and orthogonal partial least squares discrimination analysis (OPLS-DA). This is the first time to report the volatile components of H. pedunculosum, which not only find characteristic difference between female and male buds, but also point out the correlation between volatile compounds, floral odor, and plant physiology. This study enriches the basic theory of dioecious plants and has guiding significance for the production and development of H. pedunculosum germplasm resources. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)
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13 pages, 2547 KiB  
Article
Optimization of Extraction Conditions and Characterization of Volatile Organic Compounds of Eugenia klotzschiana O. Berg Fruit Pulp
by Ana P. X. Mariano, Ana L. C. C. Ramos, Afonso H. de Oliveira Júnior, Yesenia M. García, Ana C. C. F. F. de Paula, Mauro R. Silva, Rodinei Augusti, Raquel L. B. de Araújo and Júlio O. F. Melo
Molecules 2022, 27(3), 935; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27030935 - 29 Jan 2022
Cited by 8 | Viewed by 2755
Abstract
Eugenia klotzschiana O. Berg is a native species to the Cerrado biome with significant nutritional value. However, its volatile organic compounds (VOCs) chemical profile is not reported in the scientific literature. VOCs are low molecular weight chemical compounds capable of conferring aroma to [...] Read more.
Eugenia klotzschiana O. Berg is a native species to the Cerrado biome with significant nutritional value. However, its volatile organic compounds (VOCs) chemical profile is not reported in the scientific literature. VOCs are low molecular weight chemical compounds capable of conferring aroma to fruit, constituting quality markers, and participating in the maintenance and preservation of fruit species. This work studied and determined the best conditions for extraction and analysis of VOCs from the pulp of Eugenia klotzschiana O. Berg fruit and identified and characterized its aroma. Headspace solid-phase microextraction (HS-SPME) was employed using different fiber sorbents: DVB/CAR/PDMS, PDMS/DVB, and PA. Gas chromatography and mass spectrometry (GC-MS) were employed to separate, detect, and identify VOCs. Variables of time and temperature of extraction and sample weight distinctly influenced the extraction of volatiles for each fiber. PDMS/DVB was the most efficient, followed by PA and CAR/PDMS/DVB. Thirty-eight compounds that comprise the aroma were identified among sesquiterpenes (56.4%) and monoterpenes (30.8%), such as α-fenchene, guaiol, globulol, α-muurolene, γ-himachalene, α-pinene, γ-elemene, and patchoulene. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)
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10 pages, 1371 KiB  
Article
Risk Assessment of Passive Smoking Based on Analysis of Hair Nicotine and Cotinine as Exposure Biomarkers by In-Tube Solid-Phase Microextraction Coupled On-Line to LC-MS/MS
by Hiroyuki Kataoka, Sanae Kaji and Maki Moai
Molecules 2021, 26(23), 7356; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26237356 - 03 Dec 2021
Cited by 7 | Viewed by 2178
Abstract
Passive smoking due to environmental tobacco smoke is a serious public health concern because it increases the risk of lung cancer and cardiovascular disease. However, the current status and effect of passive smoking in various lifestyles are not fully understood. In this study, [...] Read more.
Passive smoking due to environmental tobacco smoke is a serious public health concern because it increases the risk of lung cancer and cardiovascular disease. However, the current status and effect of passive smoking in various lifestyles are not fully understood. In this study, we measured hair nicotine and cotinine levels as exposure biomarkers in non-smokers and assessed the risk from the actual situation of passive smoking in different lifestyle environments. Nicotine and cotinine contents in hair samples of 110 non-smoker subjects were measured by in-tube solid-phase microextraction with on-line coupling to liquid chromatography-tandem mass spectrometry, and self-reported lifestyle questionnaires were completed by the subjects. Nicotine and cotinine were detected at concentrations of 1.38 ng mg−1 and 12.8 pg mg−1 respectively in the hair of non-smokers, with levels significantly higher in subjects who reported being sensitive to tobacco smoke exposure. These levels were also affected by type of food intake and cooking method. Nicotine and cotinine in hair are useful biomarkers for assessing the effects of passive smoking on long-term exposure to environmental tobacco smoke, and our analytical methods can measure these exposure levels in people who are unaware of passive smoking. The results of this study suggest that the environment and places of tobacco smoke exposure and the lifestyle behaviors therein are important for the health effects of passive smoking. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)
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10 pages, 2587 KiB  
Article
Headspace Solid-Phase Microextraction/Gas Chromatography–Mass Spectrometry for the Determination of 2-Nonenal and Its Application to Body Odor Analysis
by Keita Saito, Yoshiyuki Tokorodani, Chihiro Sakamoto and Hiroyuki Kataoka
Molecules 2021, 26(19), 5739; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26195739 - 22 Sep 2021
Cited by 9 | Viewed by 2189
Abstract
The odors and emanations released from the human body can provide important information about the health status of individuals and the presence or absence of diseases. Since these components often emanate from the body surface in very small quantities, a simple sampling and [...] Read more.
The odors and emanations released from the human body can provide important information about the health status of individuals and the presence or absence of diseases. Since these components often emanate from the body surface in very small quantities, a simple sampling and sensitive analytical method is required. In this study, we developed a non-invasive analytical method for the measurement of the body odor component 2-nonenal by headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry by selective ion monitoring. Using a StableFlex PDMS/DVB fiber, 2-nonenal was efficiently extracted and enriched by fiber exposition at 50 °C for 45 min and was separated within 10 min using a DB−1 capillary column. Body odor sample was easily collected by gauze wiping. The limit of detection of 2-nonenal collected in gauze was 22 pg (S/N = 3), and the linearity was obtained in the range of 1–50 ng with a correlation coefficient of 0.991. The method successfully analyzed 2-nonenal in skin emissions and secretions and was applied to the analysis of body odor changes in various lifestyles, including the use of cosmetics, food intake, cigarette smoking, and stress load. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)
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13 pages, 1525 KiB  
Article
Chemical Physical Characterization and Profile of Fruit Volatile Compounds from Different Accesses of Myrciaria floribunda (H. West Ex Wild.) O. Berg through Polyacrylate Fiber
by Yesenia Mendoza García, Ana Luiza Coeli Cruz Ramos, Ana Cardoso Clemente Filha Ferreira de Paula, Maicon Heitor do Nascimento, Rodinei Augusti, Raquel Linhares Bello de Araújo, Eurico Eduardo Pinto de Lemos and Júlio Onésio Ferreira Melo
Molecules 2021, 26(17), 5281; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26175281 - 31 Aug 2021
Cited by 9 | Viewed by 2127
Abstract
Among the many species of native fruit of Brazil that have been little explored, there is Myrciaria floribunda (also known as rumberry, cambuizeiro, or guavaberry), a species with significant variability, which has fruits of different colors (orange, red, and purple) when ripe. The [...] Read more.
Among the many species of native fruit of Brazil that have been little explored, there is Myrciaria floribunda (also known as rumberry, cambuizeiro, or guavaberry), a species with significant variability, which has fruits of different colors (orange, red, and purple) when ripe. The physical-chemical characteristics evaluated were fruit weight (FW), seed weight (SW), pulp weight (PW), number of seeds (NS), longitudinal diameter (LD), transverse diameter (TD), format (LD/TD), hydrogen potential (pH), soluble solids (SS), titratable acidity (TA), and ratio (SS/TA); further, the volatile organic compounds (VOCs) of nine accesses of rumberry orchards were identified. The averages of the variables FW, SW, PW, NS, LD, TD, shape, and firmness were 0.76 g, 0.22 g, 0.54 g, 1.45, 10.06 mm, 9.90 mm, 1.02, 2.96 N, respectively. LD/TD data showed that the fruits have a slightly rounded shape (LD/TD = 1). The averages for pH, SS, TA, and SS/TA were 3.74, 17.58 Brix, 4.31% citric acid, and 4.31, respectively. The evaluated parameters indicated that the fruits can be consumed both in natura and industrialized, with the red-colored fruits presenting a good balance of SS/TA, standards demanded by the processing industries. Thirty-six VOCs were identified, with emphasis on the sesquiterpenes. Caryophyllene (21.6% to 49.3%) and γ-selinene (11.3% to 16.3%) were the most predominant compounds in rumberry fruits. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)
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12 pages, 1519 KiB  
Article
Metabolic Evaluation of Urine from Patients Diagnosed with High Grade (HG) Bladder Cancer by SPME-LC-MS Method
by Kamil Łuczykowski, Natalia Warmuzińska, Sylwia Operacz, Iga Stryjak, Joanna Bogusiewicz, Julia Jacyna, Renata Wawrzyniak, Wiktoria Struck-Lewicka, Michał J. Markuszewski and Barbara Bojko
Molecules 2021, 26(8), 2194; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26082194 - 11 Apr 2021
Cited by 19 | Viewed by 2885
Abstract
Bladder cancer (BC) is a common malignancy of the urinary system and a leading cause of death worldwide. In this work, untargeted metabolomic profiling of biological fluids is presented as a non-invasive tool for bladder cancer biomarker discovery as a first step towards [...] Read more.
Bladder cancer (BC) is a common malignancy of the urinary system and a leading cause of death worldwide. In this work, untargeted metabolomic profiling of biological fluids is presented as a non-invasive tool for bladder cancer biomarker discovery as a first step towards developing superior methods for detection, treatment, and prevention well as to further our current understanding of this disease. In this study, urine samples from 24 healthy volunteers and 24 BC patients were subjected to metabolomic profiling using high throughput solid-phase microextraction (SPME) in thin-film format and reversed-phase high-performance liquid chromatography coupled with a Q Exactive Focus Orbitrap mass spectrometer. The chemometric analysis enabled the selection of metabolites contributing to the observed separation of BC patients from the control group. Relevant differences were demonstrated for phenylalanine metabolism compounds, i.e., benzoic acid, hippuric acid, and 4-hydroxycinnamic acid. Furthermore, compounds involved in the metabolism of histidine, beta-alanine, and glycerophospholipids were also identified. Thin-film SPME can be efficiently used as an alternative approach to other traditional urine sample preparation methods, demonstrating the SPME technique as a simple and efficient tool for urinary metabolomics research. Moreover, this study’s results may support a better understanding of bladder cancer development and progression mechanisms. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)
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16 pages, 1310 KiB  
Article
Magnetic Micro-Solid-Phase Extraction Using a Novel Carbon-Based Composite Coupled with HPLC–MS/MS for Steroid Multiclass Determination in Human Plasma
by Andrea Speltini, Francesca Merlo, Federica Maraschi, Giorgio Marrubini, Anna Faravelli and Antonella Profumo
Molecules 2021, 26(7), 2061; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26072061 - 03 Apr 2021
Cited by 7 | Viewed by 2333
Abstract
A micron-sized sorbent, Magn-Humic, has been prepared by humic acids pyrolysis onto silica-coated magnetite. The material was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), thermogravimetric analysis (TGA), and Brunauer, Emmett, and Teller (BET) surface area measurements [...] Read more.
A micron-sized sorbent, Magn-Humic, has been prepared by humic acids pyrolysis onto silica-coated magnetite. The material was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), thermogravimetric analysis (TGA), and Brunauer, Emmett, and Teller (BET) surface area measurements and applied for simultaneous magnetic solid-phase extraction (MSPE) of glucocorticoids, estrogens, progestogens, and androgens at ng mL−1 levels from human plasma followed by high-performance liquid chromatography coupled with mass spectrometry (HPLC–MS/MS). Due to the low affinity for proteins, steroids extraction was done with no need for proteins precipitation/centrifugation. As highlighted by a design of experiments, MSPE was performed on 250 µL plasma (after 1:4 dilution) by 50 mg Magn-Humic (reusable for eight extractions) achieving quantitative recovery and satisfying clean-up. This was improved by washing (2 mL 2% v/v formic acid) prior to analytes elution by 0.5 mL 1:1 v/v methanol-acetonitrile followed by 0.5 mL methanol; eluate reduction to 0.25 mL compensated the initial sample dilution. The accuracy was assessed in certified blank fetal bovine serum and in human plasma, gaining satisfactory recovery in the range 65–122%, detection limits in the range 0.02–0.3 ng mL−1 (0.8 ng mL−1 for 17-β-estradiol) and suitable inter-day precision (relative standard deviation (RSD) <14%, n = 3). The method was evaluated in terms of selectivity, sensitivity, matrix-effect, instrumental carry-over, and it was applied to human plasma samples. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)
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9 pages, 902 KiB  
Article
Online In-Tube Solid-Phase Microextraction Coupled to Liquid Chromatography–Tandem Mass Spectrometry for the Determination of Tobacco-Specific Nitrosamines in Hair Samples
by Atsushi Ishizaki and Hiroyuki Kataoka
Molecules 2021, 26(7), 2056; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26072056 - 03 Apr 2021
Cited by 10 | Viewed by 2011
Abstract
Active and passive smoking are serious public health concerns Assessment of tobacco smoke exposure using effective biomarkers is needed. In this study, we developed a simultaneous determination method of five tobacco-specific nitrosamines (TSNAs) in hair by online in-tube solid-phase microextraction (SPME) coupled to [...] Read more.
Active and passive smoking are serious public health concerns Assessment of tobacco smoke exposure using effective biomarkers is needed. In this study, we developed a simultaneous determination method of five tobacco-specific nitrosamines (TSNAs) in hair by online in-tube solid-phase microextraction (SPME) coupled to liquid chromatography-tandem mass spectrometry (LC–MS/MS). TSNAs were extracted and concentrated on Supel-Q PLOT capillary by in-tube SPME and separated and detected within 5 min by LC–MS/MS using Capcell Pak C18 MGIII column and positive ion mode multiple reaction monitoring systems. These operations were fully automated by an online program. The calibration curves of TSNAs showed good linearity in the range of 0.5–1000 pg mL–1 using their stable isotope-labeled internal standards. Moreover, the limits of detection (S/N = 3) of TSNAs were in the range of 0.02–1.14 pg mL–1, and intra-day and inter-day precisions were below 7.3% and 9.2% (n = 5), respectively. The developed method is highly sensitive and specific and can easily measure TSNA levels using 5 mg hair samples. This method was used to assess long-term exposure levels to tobacco smoke in smokers and non-smokers. Full article
(This article belongs to the Special Issue Solid-Phase Microextraction and Related Techniques in Bioanalysis)
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