Separations

Research

14 pages, 1525 KiB

Open AccessArticle

Examination of Volatile Signatures of Fusarium Bulb Rot in Garlic Using Proton-Transfer-Reaction Time-of-Flight Mass Spectrometry and Solid-Phase Microextraction Gas Chromatography/Mass Spectrometry

by Alessandro Infantino, Cosimo Taiti, Alessandro Grottoli, Stefano Mancuso, Corrado Costa and Stefania Garzoli

Separations 2023, 10(11), 556; https://doi.org/10.3390/separations10110556 - 31 Oct 2023

Viewed by 1287

Abstract

Fusarium bulb rot, caused by Fusarium proliferatum, is a worldwide disease of garlic, both in the open field and during storage. Early diagnosis of the disease during storage is difficult due to the morphology of the bulbs and cloves. Volatile organic compounds [...] Read more.

Fusarium bulb rot, caused by Fusarium proliferatum, is a worldwide disease of garlic, both in the open field and during storage. Early diagnosis of the disease during storage is difficult due to the morphology of the bulbs and cloves. Volatile organic compounds (VOCs) are secondary metabolites produced by several microorganisms, including phytopathogenic fungi and bacteria. In recent years, the development of several techniques for the detection and characterization of VOCs has prompted their use, among others, as a diagnostic tool for the early and non-destructive analysis of many diseases of species of agricultural interest. In this paper, proton-transfer-reaction time-of-flight mass spectrometry (PTR-ToF-MS) and solid-phase microextraction gas chromatography/mass spectrometry (SPME-GC/MS) were successfully utilized to characterize the volatolome of commercial garlic cloves, artificially and naturally infected with F. proliferatum, for the early discrimination between diseased and healthy ones. A partial least squares discriminant analysis (PLSDA) and a principal component analysis (PCA) allowed for the separation of infected and healthy cloves and the identification of specific VOCs produced by the fungus during the infection. The results obtained in this work could be utilized for the development of simpler, more economical, and more portable devices for the early detection of infected garlic bulbs during storage. Full article

(This article belongs to the Special Issue Application of Chromatography in Analytical Chemistry)

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10 pages, 639 KiB

Open AccessArticle

Determining Polycyclic Aromatic Compounds in Bird Feathers Using Pressurized Fluid Extraction

by Vida Moradi, Thor Halldorson, Zhe Xia, Nipuni Vitharana, Chris Marvin, Philippe J. Thomas, Manon Sorais, Glenn T. Crossin and Gregg Tomy

Separations 2023, 10(9), 503; https://doi.org/10.3390/separations10090503 - 14 Sep 2023

Viewed by 943

Abstract

Due to their ease of collecting and transporting from the field and their ability to accumulate pollutants, bird feathers are increasingly being used as a non-invasive biomonitoring tool for environmental monitoring programs. Polycyclic aromatic compounds (PACs) are a diverse class of environmental pollutants, [...] Read more.

Due to their ease of collecting and transporting from the field and their ability to accumulate pollutants, bird feathers are increasingly being used as a non-invasive biomonitoring tool for environmental monitoring programs. Polycyclic aromatic compounds (PACs) are a diverse class of environmental pollutants, and because of their deleterious impacts on biological species, monitoring these compounds in wildlife is of high importance. Current approaches to measuring PACs in bird feathers involve a time-consuming acid treatment with a concomitant solvent extraction step. Here, a validated method for measuring a suite of PACs in bird feathers using pressurized fluid extraction and identification and quantitation by gas chromatography-tandem mass spectrometry is presented. Chicken (Gallus domesticus) feathers were purposely fortified with a suite of 34 PACs separately at three fortification levels and placed inside a pressurized fluid extraction cell containing silica gel/deactivated alumina to provide in situ clean-up of the sample. Except for anthracene and naphthalene, the accuracy of our method ranged for PAHs from 70–120% (irrespective of fortification level), and our intra- and inter-day repeatability was smaller than 28%. For APAHs, our accuracies ranged from 38–158%, and the inter- and intra-day repeatability was less than 35%. Our limits of detection and quantitation for both groups of compounds ranged from 0.5–13 and 1.5–44.3 ng/g, respectively. Overall, the developed method represents an effective and efficient approach for the extraction and quantitation of PACs from bird feathers that negated the need for the time-consuming and potentially harmful acid treatment. Full article

(This article belongs to the Special Issue Application of Chromatography in Analytical Chemistry)

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9 pages, 948 KiB

Open AccessArticle

A New Sample Processing Protocol for Separation and Purification Enabling Precise Analysis of Various Non-Traditional Isotopes in Geological Samples with Low Concentrations

by Jianye Gui and Wei Zou

Separations 2023, 10(9), 497; https://doi.org/10.3390/separations10090497 - 12 Sep 2023

Viewed by 818

Abstract

Many non-traditional isotopes, such as chlorine, magnesium, calcium, etc., are widely used as groundwater tracers. A new sample processing protocol of purification and concentration for isotopic analysis is presented to overcome many of the major drawbacks of existing methods. Contemporary sample preparation often [...] Read more.

Many non-traditional isotopes, such as chlorine, magnesium, calcium, etc., are widely used as groundwater tracers. A new sample processing protocol of purification and concentration for isotopic analysis is presented to overcome many of the major drawbacks of existing methods. Contemporary sample preparation often requires several laborious off-line procedures in a ultra clean laboratory prior to instrumental determination; additionally, interference ions in real samples are difficult to completely remove, especially when the concentration of those ions is equal to that of the target ions. The new protocol includes the following steps: (i) one-step purification using a newly developed isotopic preparative chromatograph (IPC) with a background suppressed mode to obtain extremely pure components that only have target ions and H₂O; (ii) enrichment of the collected pure solution from the previous step using a newly developed ultra clean concentrator filled with high purity nitrogen; (iii) transforming the enriched target ion into suitable speciation inside the ultra clean concentrator; (iv) finally, sending the enriched solutions to a multi-collector inductively coupled-plasma mass-spectrometer (MC-ICP-MS) or thermal ionization mass spectrometer (TIMS). The present method was validated using certified reference materials and real samples for both chlorine and magnesium; the precision of chlorine ratio value was generally below 0.22‰ and that of Mg was below 0.12‰. This processing protocol provides a potential method for isotope sample preparation and analysis in a small number of geological samples with low concentrations of many other elements or compounds such as nitrate, sulfate, lithium, calcium, strontium, etc. Full article

(This article belongs to the Special Issue Application of Chromatography in Analytical Chemistry)

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17 pages, 2273 KiB

Open AccessEditor’s ChoiceArticle

Characterization of the Aroma Profile of Food Smoke at Controllable Pyrolysis Temperatures

by Marina Rigling, Laura Höckmeier, Malte Leible, Kurt Herrmann, Monika Gibis, Jochen Weiss and Yanyan Zhang

Separations 2023, 10(3), 176; https://doi.org/10.3390/separations10030176 - 06 Mar 2023

Cited by 3 | Viewed by 1813

Abstract

Smoking is used to give food its typical aroma and to obtain the desired techno-functional properties of the product. To gain a deeper knowledge of the whole process of food smoking, a controllable smoking process was developed, and the influence of wood pyrolysis [...] Read more.

Smoking is used to give food its typical aroma and to obtain the desired techno-functional properties of the product. To gain a deeper knowledge of the whole process of food smoking, a controllable smoking process was developed, and the influence of wood pyrolysis temperature (150–900 °C) on the volatile compounds in the smoking chamber atmosphere was investigated. The aroma profile of smoke was decoded by headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS). Subsequently, the correlations in the most important substance classes, as well as in individual target components, were investigated by the Pearson test. Phenols and lactones showed an increase over the entire applied temperature range (r_T = 0.94 and r_T = 0.90), whereas furans and carbonyls showed no strict temperature dependence (r_T < 0.6). Investigations on single aroma compounds showed that not all compounds of one substance class showed the same behavior, e.g., guaiacol showed no significant increase over the applied pyrolysis temperature, whereas syringol and hydoxyacetone showed a plateau after 450 °C, and phenol and cyclotene increased linear over the applied temperature range. These findings will help to better understand the production of aroma-active compounds during smoke generation in order to meet consumers preferences. Full article

(This article belongs to the Special Issue Application of Chromatography in Analytical Chemistry)

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10 pages, 4008 KiB

Open AccessArticle

Thin Layer Chromatographic Method for Detection of Conventional Drug Adulterants in Herbal Products

by Christopher Johnson Mwankuna, Eliapenda Elisante Mariki, Faith Philemon Mabiki, Hamisi Masanja Malebo, Bjarne Styrishave and Robinson Hammerton Mdegela

Separations 2023, 10(1), 23; https://doi.org/10.3390/separations10010023 - 31 Dec 2022

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Abstract

Commercially available conventional drugs have been used to adulterate herbal products. Considering the rapid growth of herbal products’ market, it is essential to screen herbal products for the presence of conventional drugs. Simple analytical methods are needed for the rapid screening of conventional [...] Read more.

Commercially available conventional drugs have been used to adulterate herbal products. Considering the rapid growth of herbal products’ market, it is essential to screen herbal products for the presence of conventional drugs. Simple analytical methods are needed for the rapid screening of conventional drugs that are likely to be adulterated in herbal products. Thin layer chromatography (TLC) methods for screening twelve conventional drugs in herbal products have been developed and applied. The analytes were extracted from herbal products using acetonitrile:methanol:acetic acid:water (4:4:1:1, v/v). Solvent mixture of dichloromethane:ethyl acetate:methanol (75:15:10, v/v) separated well trimethoprim, sildenafil, paracetamol, and sulfamethoxazole while pyrimethamine, metronidazole, and sulfadoxine were well separated by dichloromethane:ethyl acetate:methanol (77.5:12.5:10, v/v). In addition, acetyl salicylic acid, ibuprofen, diclofenac, quinine, and lumefantrine were well separated by ethyl acetate:methanol:30% ammonia (75:22.5:2.5, v/v). Chromatographic separations were found to be highly reproducible, and more than 10 samples can be analysed in one run. The method was applied in the screening of 229 herbal products. Consequently, 24.0% of the samples contained one adulterant, while 21.4% contained at least two adulterants. All conventional drugs detected in herbal products were not mentioned on the labels and therefore the consumers are kept unaware of their side effects and health problems. Further studies for confirming and quantitatively determining the adulterants in a wide range of products as well as a systematic toxicological analysis of the adulterants in herbal products are recommended. Full article

(This article belongs to the Special Issue Application of Chromatography in Analytical Chemistry)

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9 pages, 999 KiB

Open AccessArticle

Phytochemical Compound Profile and the Estimation of the Ferruginol Compound in Different Parts (Roots, Leaves, and Seeds) of Juniperus procera

by Abdalrhaman M. Salih, Fahad Al-Qurainy, Mohamed Tarroum, Salim Khan, Mohammad Nadeem, Hassan O. Shaikhaldein and Saleh Alansi

Separations 2022, 9(11), 352; https://doi.org/10.3390/separations9110352 - 07 Nov 2022

Cited by 4 | Viewed by 1543

Abstract

Secondary plant metabolites and their derivatives play a significant role in human health. Ferruginol is a diterpene phenol that has recently received attention for its pharmacological properties, including antibacterial, antitumor, antimalarial, and cardioprotective effects. Recently, we detected the ferruginol compound in the leaf [...] Read more.

Secondary plant metabolites and their derivatives play a significant role in human health. Ferruginol is a diterpene phenol that has recently received attention for its pharmacological properties, including antibacterial, antitumor, antimalarial, and cardioprotective effects. Recently, we detected the ferruginol compound in the leaf and seed extracts of Juniperus procera using different analytical approaches. The present work aims at detecting phytochemical compounds in a root extract of J. procera and estimating the amount of ferruginol compound in different parts of Juniperus procera. To screen the phytochemical compounds present in the root extract of J. procera, Gas chromatography/mass spectrometry (GC/MS) was performed. For ferruginol identification and estimation, high-performance liquid chromatography (HPLC) with the ferruginol reference standard and high-resolution direct analysis in real-time (DART) time-of-flight mass spectrometry (TOFMS) (DART-TOF-MS) analysis were used. GC/MS analysis revealed more than 20 bioactive compounds related to secondary plant metabolites in the root extract of J. procera with biological activity. The DART-TOF-MS result showed the typical positive ion spectra of ferruginol, and the HPLC result confirmed that the root extract of J. procera contains the ferruginol compound. In contrast, the root extract of J. procera contained a significant amount of ferruginol compared to that in the leaf and seed extracts. All parts of the J. procera contained the ferruginol compound and proved that ferruginol might be accumulated in the roots, leaves, and seeds of J. procera. Full article

(This article belongs to the Special Issue Application of Chromatography in Analytical Chemistry)

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12 pages, 767 KiB

Open AccessArticle

Two Eco-Friendly Chromatographic Methods Evaluated by GAPI for Simultaneous Determination of the Fluoroquinolones Moxifloxacin, Levofloxacin, and Gemifloxacin in Their Pharmaceutical Products

by Eman A. Abdel Hameed, Zaitona A. Abd El-Naby, Alaa El Gindy, Roshdy E. Saraya, Aisha Nawaf Al balawi, Sawsan A. Zaitone and Gasser M. Khairy

Separations 2022, 9(11), 330; https://doi.org/10.3390/separations9110330 - 28 Oct 2022

Cited by 4 | Viewed by 1479

Abstract

In this paper, novel green HPLC and HPTLC chromatographic methods were developed for the concurrent determination of moxifloxacin, levofloxacin, and gemifloxacin in bulk and pharmaceutical products. The green HPLC method was used on Thermo C18 (4.6 × 250 mm, 5 µm). By mixing [...] Read more.

In this paper, novel green HPLC and HPTLC chromatographic methods were developed for the concurrent determination of moxifloxacin, levofloxacin, and gemifloxacin in bulk and pharmaceutical products. The green HPLC method was used on Thermo C18 (4.6 × 250 mm, 5 µm). By mixing ethanol and 20 mM sodium dihydrogen phosphate dihydrate (pH 5) in a ratio of 25:75, v/v, the mobile phase was created using isocratic elution. The flow rate was 1 mLmin⁻¹. The studied antibiotics were separated well within 9.5 min. The green HPTLC method was used on coated HPTLC aluminum sheets with Silica gel 60 F254 using a mobile phase mixture of water: acetone: ammonia (8:1:1, v/v/v). Compact and well-resolved peaks were obtained under chamber-saturation circumstances for the standard fluoroquinolone antibiotics. Both methods were optimized individually, validated by ICH, and assessed using the Green analytical procedure index (GAPI). The methods were applied to pharmaceutical products and compared with the published methods for the determination of each of these antibiotics individually, using Student’s t-test. They can be used by quality-control laboratories in pharmaceutical factories as sensitive eco-friendly methods for the analysis of these drugs and for the detection of cross-contamination during manufacturing processes. Full article

(This article belongs to the Special Issue Application of Chromatography in Analytical Chemistry)

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11 pages, 1197 KiB

Open AccessArticle

Two New HPLC Methods, Assessed by GAPI, for Simultaneous Determination of Four Antipsychotics in Pharmaceutical Formulations: A Comparative Study

by Eman A. Abdel Hameed, Zaitona A. Abd El-Naby, Alaa El Gindy, Sawsan A. Zaitone, Reem Alshaman, Roshdy E. Saraya and Gasser M. Khairy

Separations 2022, 9(8), 220; https://doi.org/10.3390/separations9080220 - 15 Aug 2022

Cited by 5 | Viewed by 2130

Abstract

Antipsychotics are widely used to treat various mental disorders. Combination therapies were approved by the FDA to treat manic states. Quetiapine fumarate, aripiprazole, asenapine maleate, and chlorpromazine HCl are frequently used for treatment of these disorders. Green analytical chemistry is primarily concerned with [...] Read more.

Antipsychotics are widely used to treat various mental disorders. Combination therapies were approved by the FDA to treat manic states. Quetiapine fumarate, aripiprazole, asenapine maleate, and chlorpromazine HCl are frequently used for treatment of these disorders. Green analytical chemistry is primarily concerned with reducing waste generated during sample preparation or analysis. Green solvents, such as ethanol, are being used in HPLC as an alternative to acetonitrile. To this purpose, two new chromatographic methods were developed to determine these four drugs simultaneously in their bulk and pharmaceutical formulations. The greenness of both methods was assessed by the green analytical procedure index (GAPI)—one of them was found to be green ecofriendly, and the other had some environmental hazards (conventional)—and this helps laboratories to choose a method that suits their capabilities. The chromatographic separation for both methods was carried out on a Thermo^® C18 column. The total separation times were about 11 min and 9 min for the green and the conventional methods, respectively. Using the Student’s t-test and the F-ratio, there was no significant difference between the results of the two methods. These methods have been validated and successfully applied to the analysis of commercial pharmaceutical formulations. Our study could successfully be used in central quality control laboratories, which need a single analytical method to separate more than one compound with similar pharmacological action. Full article

(This article belongs to the Special Issue Application of Chromatography in Analytical Chemistry)

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