Separations

The date palm has been cultivated in dry and hot areas of the planet for much of human history. In the Kingdom of Saudi Arabia, dates are the main crop used as a source of food. Among several species of date fruits, the Ajwa AL-Madinah date is unique, growing only in Al-Madinah geographical region. The Ajwa date is used in traditional medicine due to its abundant active components and therapeutic properties. This study investigates the structural properties and the antioxidant effects of water-soluble polysaccharides extracted from Ajwa flesh and seed. The polysaccharides were isolated by two techniques including hot water and ultrasonic extraction. After isolation and partial purification, the physicochemical properties of four samples of polysaccharides extracted from flesh and seed were studied by several techniques including FTIR, solid-state NMR, elemental analysis, and mass spectrometry. Several radical scavenging experiments were combined to study the antioxidant activity of the polysaccharide compounds. FTIR and NMR results showed a structure typical of heterogeneous polysaccharides. Mass spectrometry revealed that the polysaccharide samples were composed mainly of mannose, glucose, galactose, xylose, arabinose, galacturonic acid, and fucose. In addition, the physicochemical properties and composition of polysaccharides extracted from flesh and seed were compared. The extracted polysaccharides showed antioxidant activity, with 2, 2′-azinobis (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) radical scavenging, Fe chelating ability, hydroxyl free radical scavenging ability, and 2, 2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging. These results highlight their potential to be a useful nutritional element or supplemental medication. Full article

A huge number of date varieties grow annually throughout the world. The genetic variation between different date varieties is reflected in their variable sensory characters and phytochemical contents. Date pits are considered a waste product of the date industry, despite their rich metabolic content. The present study attempts to generate visual clustering to clarify the diversity among fourteen date cultivars growing in the Qassim region, according to the phytochemical contents and biological potentials of their pits. The results indicated a wide variation in the total phenolic content (11.4–29.7 mg GAE/g), flavonoids content (21.9–37.1 mg RE/g), proanthocyanidine content (12.0–207.0 mg CE/g), and antioxidant potential (10.3–25.5 mg AEAC/g) among the tested cultivars. Screening the antimicrobial activity of extracts from the 14 tested cultivars indicated different activities against Listeria monocytogenes, Staphylococcus aureus, Escherichia coli, Salmonella enterica, and Candida albicans. Multivariate analysis of phytochemical content and biological activity, using different analytical models, allowed the classification of the 14 cultivars into four classes, Class-1: Barhi, Safawi, and Sukkari; Class-2: Khodry and Nabtat Ali; Class-3: Ruthana, Segae, Shaqra, and Sheishee; and Class-4: Hulwa Aljouf, Mabroom, Meneifi, Rushodia, and Wannana. These findings provide a scientific basis for the classification of date pits which facilitates the future selection of promising candidates for more phytochemical and biological exploration. Full article

Microplastic-derived dissolved organic matter (MP-DOM) has received increasing attention in recent years. In this study, the fluorescence excitation-emission matrix (EEM) combined with parallel factor analysis (PARAFAC) was used to track the leaching behavior of polyethylene (PE), polyvinyl chloride (PVC), polypropylene (PP), polyethylene terephthalate (PET), and polystyrene (PS) MP-DOM. After seven days of leaching, PVC reached a leaching concentration of 7.59 mg/L, and the other four microplastics reached approximately 4.5~4.7 mg/L. The leaching activity of PVC was considerably more active in an alkaline environment and under UV irradiation. All the fluorescence signals of MP-DOM components were located in the protein/phenol-like fluorescence region. The fact that C1 and C2 were found in every microplastic revealed that these substances took up quite a large proportion of MP-DOM. Protein/phenolic substances in MP-DOM showed different binding ability with different heavy metals, which can be realized from the log K values calculated for Cr³⁺ (3.99–5.51), Cu²⁺ (3.06–4.83), Cd²⁺ (3.76–4.41), and Fe³⁺ (3.11–5.03). This work introduced more MP-DOM samples, and offered spectroscopic insight into the characteristics and environmental fate of MP-DOM at a molecular level. Furthermore, this study displayed the potential applicability of using the integrated methods to track the MP-DOM formation process and environmental behavior in natural aquatic systems. Full article

Essential oils (EOs) have recently attracted more interest due to their insecticidal activities, low harmfulness, and rapid degradation in the environment. Therefore, Lavandula steochas (L. steochas) essential oil was assessed for its chemical constituents, in vitro cytotoxicity, and scolicidal, acaricidal, and insecticidal activities. Using spectrometry and gas chromatography, the components of L. steochas EOs were detected. Additionally, different oil concentrations were tested for their anticancer activities when applied to human embryonic kidney cells (HEK-293 cells) and the human breast cancer cell line MCF-7. The oil’s scolicidal activity against protoscolices of hydatid cysts was evaluated at various concentrations and exposure times. The oil’s adulticidal, larvicidal, and repelling effects on R. annulatus ticks were also investigated at various concentrations, ranging from 0.625 to 10%. Likewise, the larvicidal and pupicidal activities of L. steochas against Musca domestica were estimated at different concentrations. The analyses of L. steochas oil identified camphor as the predominant compound (58.38%). L. steochas oil showed significant cytotoxicity against cancer cells. All of the tested oil concentrations demonstrated significant scolicidal activities against the protoscoleces of hydatid cysts. L. steochas EO (essential oil) showed 100% adulticidal activity against R. annulatus at a 10% concentration with an LC₅₀ of 2.34%, whereas the larvicidal activity was 86.67% and the LC₅₀ was 9.11%. On the other hand, the oil showed no repellent activity against this tick’s larva. Furthermore, L. steochas EO achieved 100% larvicidal and pupicidal effects against M. domestica at a 10% concentration with LC₅₀ values of 1.79% and 1.51%, respectively. In conclusion, the current work suggests that L. steochas EO could serve as a potential source of scolicidal, acaricidal, insecticidal, and anticancer agents. Full article

An ion chromatography technique with conductivity detection was selected as an analytical tool for the simultaneous indirect determination of sodium sulfate, potassium sulfate, and magnesium sulfate via their respective cations. The method was developed and validated for the quantitative assay of the inorganic salts under study in oral pharmaceutical dosage forms. Chromatographic separation was achieved on a Dionex^®IonPac^® CS16 column (250 × 5 mm) column using the gradient elution method. A mobile phase-A consisting of methane sulfonic acid (6.7%, v/v) in Milli-Q water, which is used together with Milli-Q water, was used as a mobile Phase-B. The flow rate was 1.2 mL/min. The retention times of sodium, potassium, and magnesium as sulfates were 7.8, 12.8, and 16.2 min, respectively. The method was validated according to ICH guidelines and showed good linearity and accuracy results within concentration ranges of 80.0–240.0, 20.0–60.0, and 4.5–13.5 ppm for sodium, potassium, and magnesium as sulfates, respectively. The relative standard deviation results for intra- and inter-day precision were less than 1.0%. The method was applied successfully for determination of the analytes under study in their mixed pharmaceutical oral solution and found suitable for their routine and stability analysis. Full article

Despite the fact that several analytical methodologies have been reported for the determination of curcumin (CCM) in a wide range of sample matrices, the greener liquid chromatographic approaches to determine CCM are scarce in the literature. Therefore, this research is designed to develop and validate a greener stability-indicating “high-performance liquid chromatography (HPLC)” methodology to determine CCM in an in-house developed nanoemulsion, Curcuma longa L. extract, and commercial tablets. CCM was measured on a Nucleodur (150 mm × 4.6 mm) RP C₁₈ column with 5 µm-sized particles. Ethanol and ethyl acetate (83:17 v/v) made up the greener eluent system, which was pumped at a flow speed of 1.0 mL/min. At a wavelength of 425 nm, CCM was detected. The greener HPLC methodology was linear in the 1–100 µg/mL range, with a determination coefficient of 0.9983. The greener HPLC methodology for CCM estimation was also rapid (R_t = 3.57 min), accurate (%recoveries = 98.90–101.85), precise (%CV = 0.90–1.11), and sensitive (LOD = 0.39 µg/mL and LOQ = 1.17 µg/mL). The AGREE approach predicted the AGREE score of 0.81 for the established HPLC technique, indicating an outstanding greenness profile. The utility of the greener HPLC methodology was demonstrated by determining CCM in the in-house developed nanoemulsion, Curcuma longa extract, and commercial tablets. The % amount of CCM in the in-house developed nanoemulsion, Curcuma longa extract, and commercial tablets was found to be 101.24%, 81.15%, and 78.41%, respectively. The greener HPLC methodology was able to detect its degradation product under various stress conditions, suggesting its stability-indication characteristics. These results suggested that CCM in developed nanoemulsion, plant extract samples, and commercial tablets may be routinely determined using the greener HPLC methodology. Full article

It is of great necessity to develop new antimicrobial agents to overcome the accelerated increment in drug-resistant bacteria. The main aim of this work is to manufacture two cationic surfactants, QHETA-9 and QHETA-14, based on quaternary hexamethylenetetramine with long alkyl chains (C-9 and C-14) by simple one-step alkylation reaction. These surfactants were characterized by analytical and statistical data, including FTIR, ¹H NMR, ¹³C NMR and DLS. The antibacterial activities of QHETA-9 and QHETA-14 against some pathogenic bacterial strains were tested using agar disk diffusion method. The results exhibited that QHETA-14 has higher antibacterial activity than that of QHETA-9. It displayed inhibitory zone values for Staphylococcus aureus, methicillin-resistant Staphylococcus aureus (MRSA) and Enterococcus faecalis, as Gram-positive bacteria, of 22.7, 21.5 and 25.9 mm, respectively, at 200 μg/disk. Meanwhile, it recorded inhibition zone values of 17.5, 25.2 and 23.8 mm for Escherichia coli, Agrobacterium tumefaciens and Erwinia carotovora, respectively, at 200 μg/disk. As a result, the current investigation verified that the antibacterial properties of QHETA-14 were greater than those of QHETA-9 due to the increase in the length of the alkyl chain. It is clear that QHETA-14 has the potential to be used as an antibacterial agent against bacteria that cause nosocomial infections and food poisoning diseases. Full article

The potential of raw durian husk and NaOH-modified durian husk as an adsorbent, using different doses, 0.5 g, 1.0 g, 1.5 g, and 2.0 g, is investigated to improve soaking water of pepper berries during the retting process. The surface area and the pore size of the durian husk were examined using Brunner Emmett and Teller analysis. The surface area of NaOH-modified durian husk is higher (2.33 m²/g) compared to the raw durian husk (1.51 m²/g). NaOH-modified durian husk has a higher porous structure than the raw durian husk, but both pore diameters are more than 50 nm, which is considered micropore raw material. The effect of the raw durian husk on pH, chemical oxygen demand (COD), dissolved oxygen (DO), and turbidity were compared to the NaOH-modified durian husk with different doses. The 2.0 g of NaOH-modified durian husk enhanced changes in the four parameters. The highest pH value using NaOH-modified durian husk was 6.10 ± 0.02, while turbidity and COD increased to 971.33 ± 1.15 NTU and 1984.67 ± 3.21 mg/L, respectively. The DO of NaOH-modified durian husk shows the lowest reduction to 1.49 mg/L with 2.0 g of NaOH-modified durian husk. The experimental data was best fitted with a first-order kinetic model. Durian husk treated with NaOH could be used as a potential adsorbent to enhance the soaking water for pepper berries. Full article

Vanadium titanomagnetite (VTM) is an important mineral for developing titanium resources, but the comprehensive recovery of ilmenite separation is extremely poor, resulting in the low-efficiency utilization of titanium resources. Here, the separation of ilmenite from VTM ore is studied by combining magnetic separation and flotation technologies. In particular, the floatability of mixed MOH/PG-1 collectors is thoroughly investigated. The results show that a concentrate with a TiO₂ grade of 9.90% can be separated via weak magnetic separation and coarse particle tailing dumping. The concentrate grade is then increased to 14.32% via strong magnetic separation and floating separation of sulfur minerals. Finally, a TiO₂ grade of 46.34% is obtained through closed-circuit flotation using mixed MOH/PG-1 collectors. The mixed collectors are very efficient and can enhance the chemical adsorption of the Ti⁴⁺, Fe³⁺, and Fe²⁺ ions in the ilmenite concentrate compared with the MOH collector, thereby increasing the TiO₂ grade and recovery by 3.31% and 1.20%, respectively. This is beneficial for improving the comprehensive utilization of titanium resources in VTM ores. Full article

Fatty liver (FL) is one of the most prevalent diseases in the world, characterized by insulin resistance and hyperlipidemia, which consequently lead to neurodegenerative disorders through the induction of oxidative stress-inflammatory axis, which alters the neurotransmitters’ levels. Calluna vulgaris (CV), also known as heather, has anti-inflammatory and antidepressant properties, making it a promising candidate for treating steatosis and brain lesions. This study aimed to assess the prophylactic and therapeutic effect of CV extract on brain dysfunction associated with steatosis. FL was induced in rats by CCl₄ oral administration (50 µL/Kg in olive oil three times/week) for six weeks. The protection group received 200 mg/kg CV extract orally for two weeks before and two weeks during FL induction, while the treatment group was orally administered CV extract after FL induction for one month. The biochemical parameters revealed that CCl₄ administration induced hepatotoxicity as blood-liver function parameters (AST, ALT, ALP, protein, and LDH) were increased by 1.8, 1.4, 2, 2.4, and 1.2-fold, respectively. Moreover, insulin resistance was characterized by a two-fold increase in the glucose, insulin, and lipid profile when compared to control one, at p < 0.05. Steatosis liver demonstrated a two-fold increase in all following parameters— acetaldehyde (AC), prooxidant (TBARS), acetylcholine esterase (AChE), monoamine oxidase (MAO), hyaluronidase, and ATPase—when compared to control one, at p < 0.05. CCl₄ administration led to brain lesions where the brain level of TBARS, insulin, cholesterol, AChE, and MAO was progressively increased by 2, 1.6, 2.2, 4, and 1.6-fold, respectively, that was associated with reduced glucose (8-fold) and GSH (2-fold) than that of control level, at p < 0.05. CV extract as a prophylactic and therapeutic agent increased GSH and decreased TBARS of both the liver and brain than that of induced group, at p < 0.05, normalized the activities of AChE and MAO, and increased insulin sensitivity where they successfully decreased the HOMA-IR, glucose, TG, and cholesterol compared to than that of induced group, at p < 0.05. This positive effect of CV extract contributed to the presence of polyphenolic compounds such as catechins (5.501 ± 0.056 µg/g extract), gallic (3.525 ± 0.143 µg/g) extract, and protocatechuic acid (2.719 ± 0.132 µg/g extract). Therefore, we concluded that FL induced brain dysfunction through the formation of ROS and elevation of insulin and lipid inside the brain tissue, which alter the amount of neurotransmitter and cellular energy production. Rich in polyphenolic compounds, CV extract functions as an antioxidant, antidiabetic, hepatoprotective, inhibitor of neurotransmitter catabolizing enzymes, and a regulator for energy production. Therefore, it can be used as a preventative or treatment for NAFLD and brain damage. Full article

A new method of dispersive liquid-liquid microextraction (DLLME) combined with graphite furnace atomic absorption spectrometry (GFAAS) was proposed for the determination of ultra-trace copper. It was based on the reaction of Cu(II) with the laboratory-prepared chelating agent 2-(5-bromo-2-pyridylazo)-5-dimethylaminoaniline (5-Br-PADMA) in a HAc-NaAc buffer solution at pH 5.0 to form stable hydrophobic chelates, which were separated and enriched by DLLME with chlorobenzene (C₆H₅Cl) and acetonitrile (CH₃CN) as extraction and disperser solvents, respectively. The sedimented phase containing the chelates was then determined with GFAAS. Various operating variables that may be affected by the extraction process such as the pH of the solution, the concentration of the chelating agent 5-Br-PADMA, the types and volumes of extraction and disperser solvents, the extraction time, and the centrifugation time were investigated. Under optimum conditions, the calibration curve was linear in the range from 0.02 ng/mL to 0.16 ng/mL of copper with a correlation coefficient of r = 0.9961, and the detection limit was 0.01 ng/mL based on 3S_b. The relative standard deviation for six replicate measurements of 0.05 ng /mL of copper was 3.9%. An enrichment factor (EF) of 110 was obtained. The method has the advantages of low detection limit, high sensitivity, simple operation, less consumption of organic solvents, higher enrichment factor, and environmental friendliness and was applied to the determination of trace copper in environmental water samples with satisfactory results. Full article

Polyphenols are secondary metabolites of interest due to their potential application in various fields. This study is supposed to analyse the content of total polyphenols, total tannins, condensed tannins and antioxidant activity of ten wild plant species of nutritive interest to better understand their potential applications. Furthermore, the effect of heavy metals on the production of the investigated secondary metabolites was analysed. The different phenolic compounds were determined in methanol extracts obtained from edible plants collected during three sampling periods (June, September and November–December) in four areas of the Central Italy. Analyses were carried out by applying standard methodologies. In particular, total polyphenols were determined by the Folin–Ciocalteu method, total tannins by the polyvinylpolypyrrolidone (PVPP) reagent and condensed tannins by the 4-(dimethylamino)cinnamaldehyde (DMCA). Antioxidant activity was determined by assessing the scavenging capacity of 2,2-diphenyl-1-picrylhydrazyl (DPPH). The results showed a satisfactory content of phenolic compounds and antioxidant activity for all species analysed. Furthermore, the existence of a negative correlation between the presence of heavy metals and phenolic compounds was found. Results proved the potential use of these plants for balanced feeding of ruminants. Full article

In this work, the fresh leaves and inflorescences of Humulus lupulus L. cv. Chinook hops were investigated in order to describe their chemical composition and evaluate their biological activities. The analyses were carried out first on fresh untreated samples and then on pulverized ones using the SPME-GC-MS technique. In total, forty-two molecules belonging to different chemical classes were identified, and among these, twenty-three were terpene compounds. In order to carry out the activity assays, the powders were subjected to extraction with two different solvents (methanol and distilled water) by stirring and subsequent sonication at room temperature. To chemically characterize the extracts, the methanolic ones were analyzed by direct injection into the GC-MS apparatus, while the aqueous ones were analyzed by DI-SPME-GC-MS. In addition, with the aim to obtain information on the non-volatile content of the methanolic extracts, they were also subjected to derivatization, and the silylated derivatives were analyzed by GC-MS. The antioxidant activity was then evaluated by means of DPPH and ABTS assays after the determination of the total content of polyphenols and flavonoids. The greatest effects were observed on the methanolic extracts rather than on the aqueous ones. Furthermore, a preliminary study on the cytotoxic power of the methanolic extracts was also conducted on three different human cancer cell lines, such as non-small cell lung cancer (H1299), melanoma (A375) and breast cancer (MCF7). The obtained results showed that the two extracts induced a marginal effect on reducing breast tumor, melanoma and non-small cell lung cancer cell proliferation. Full article

The methods of hot water extraction and ultrasound-assisted enzymatic treatment were applied for extracting the soluble dietary fiber from the glutinous rice bran in the study. Based on the single factor experiment for the hot water method, the optimum parameters of the extraction time of 120 min, solid-liquid ratio 1:20 (w/v), and pH 8.0, as well as the extraction temperature 80 °C, were obtained, while the yield and purity of SDF reached 31.83 ± 0.06% and 93.28 ± 0.27%, respectively. Furthermore, the SDF yield was improved to 34.87 ± 0.55% by using the ultrasound-assisted enzymatic treatment under the optimum conditions of cellulase dosage 9 × 10³ U/g and ultrasonic temperature of 50 °C. Similar polysaccharide compositions were detected based on the infrared spectroscopic analysis. Compared with the SDF obtained from hot water extraction, the whiteness, solubility, water holding capacity, and swelling properties of SDF extracted by ultrasound-assisted enzymatic method improved significantly. These results demonstrated that both two strategies could be applied to SDF extraction in practical production, and the ultrasound-assisted enzymatic method might be an effective tool to improve the functional properties of SDF. Full article

Background: Dawa ul Kurkum (Duk) is a widely used Unani formulation. It consists of seven plant herbs, including stigmas of Crocus sativus L., rhizomes of Nardostachys jatamansi (D.Don) DC., the bark of Cinnamomum cassia (L.) J. Presl., shoot of Cymbopogon jwarancusa (Jones ex Roxb.) Schult., the resin of Commiphora wightii (Arn.) Bhandari, roots of Saussurea lappa (Decne.) Sch.Bip., and bark of Cinnamomum zeylanicum Blume. However, no study has been previously conducted to characterize this formulation. Thus, the present study was designed to carry out the pharmacognostic and phytochemical characterization of Duk. Methods: Duk was prepared following the protocols in Bayaz e Kabeer and The National Formulary of Unani Medicine Part-I. The characterization included organoleptic properties, fluorescence analysis, preliminary phytochemical screening, antioxidant activity, and active constituent profiling using HPTLC. Results: Evaluation of Duk showed the presence of carbohydrates, flavonoids, quinones, glycosides, cardiac glycosides, terpenoids, phenols, coumarin, steroids, and phytosterols. The total phenolic and flavonoid content was 5.75 ± 0.23 mg GAE/g and 10 ± 0.18 mg QUE/g, respectively. HPTLC of Duk showed the presence of p-coumaric acid, cinnamaldehyde, citral, crocin, isovaleric acid, guggulsterone, and dehydrocostus lactone. Conclusions: Our findings supported the use of Duk as a conventional medicine, and these results could be used as a reference for the standardization of Duk. Full article

Cd(II) and Cu(II) ions cause many diseases in humans. Therefore, they should be removed from water sources using simple and cost-effective adsorbents. Consequently, sodium magnesium silicate hydroxide/sodium magnesium silicate hydrate nanostructures were synthesized and functionalized using 2,3-dihydroxybenzaldehyde as a novel nanocomposite. Several instruments were used to characterize the synthetic products, such as an X-ray diffractometer (XRD), a Fourier-transform infrared spectrophotometer (FT-IR), an N₂ adsorption/desorption analyzer, a CHN elemental analyzer, an energy-dispersive X-ray spectrophotometer (EDS), and a field emission scanning electron microscope (FE-SEM). The functionalization of the nanostructures with 2,3-dihydroxybenzaldehyde led to the disappearance of the XRD peaks of the nanostructures and the presence of a broad XRD peak at 2θ = 32°. In addition, the FE-SEM images revealed that the nanostructures consisted of spheres, cubes, and irregular shapes with an average grain size of 115 nm, and the nanocomposite consisted of spherical conglomerates consisting of needle-like shapes. The anticipated morphology following the functionalization of the nanostructures with 2,3-dihydroxybenzaldehyde resulted from the presence of 2,3-dihydroxybenzaldehyde on the backbones of the nanostructures. The EDS results showed that the nanostructures were composed of O, Na, Mg, and Si with weight percentages equal to 38.59%, 5.95%, 16.60%, and 38.86%, respectively. Additionally, the nanocomposite was composed of C, N, O, Na, Mg, and Si with weight percentages equal to 55.31%, 2.23%, 30.09%, 6.56%, 2.98%, and 12.83%, respectively. The synthesized nanostructures and nanocomposite samples were utilized for the efficient removal of cadmium and copper ions from aqueous media using the ion exchange and chelation adsorption procedures, respectively. Optimum conditions for removing the cadmium and copper ions were achieved at a pH, time, and temperature equal to 7.5, 80 min, and 298 K, respectively. The maximum uptake capacities of the synthesized nanostructures and nanocomposite samples toward cadmium ions were 89.44 mg/g and 155.04 mg/g, respectively, and the maximum uptake capacities of the synthesized nanostructures and nanocomposite samples toward copper ions were 103.73 mg/g and 177.94 mg/g, respectively. Moreover, the adsorption processes were exothermic, chemical, and followed the pseudo-second-order model and Langmuir equilibrium isotherm model. Full article

Nitrated fatty acids (NO₂-FAs) are a newly discovered class of biologically active compounds with distinct biochemical features that induce physiologically beneficial alterations in transcriptional regulatory protein function, leading to a variety of modulatory and protective actions. The most common NO₂-FAs identified in vivo so far are nitro oleic acid (NO₂-OA), nitro linoleic acid (NO₂-LA) and its structural isomer nitro-conjugated linoleic acid (NO₂-cLA). Analytical limitations that compromise accurate quantitation of these endogenous compounds are their low concentrations, compromised stability and different distribution profiles in tissues and biofluids. As a result, reliable analytical methods for the quantitative determination of their endogenous levels are rare. Only NO₂-OA was quantified by GC-MS while LC-MS methods are still scarce. In this work, an LC-MS/MS bioanalytical method was developed and validated for the quantification of NO₂-OA and NO₂-LA in human plasma via a standard addition protocol after protein precipitation, liquid extraction and LC-MS/MS analysis in the negative ion mode. Quantification was performed via multiple reaction monitoring of the transitions m/z 326 > 46 and m/z 324 > 46 for NO₂-OA and NO₂-LA, respectively, and m/z 269 > 250 for the internal standard heptadecanoic acid. Linear responses were observed for both analytes over the studied range (R² = 0.9805 and 0.9644 for NO₂-OA and NO₂-LA, respectively). Sufficient accuracy and precision were also achieved at low, medium and high levels within the linearity range. The limits of quantification of our method (2 nM for both NO₂-FAs) were below basal endogenous levels, thereby providing a good tool to accurately measure these NO₂-FAs in plasma. We applied the validated method to compare NO₂-OA and NO₂-LA levels in the plasma of 28 ischemic heart disease (IHD) patients and 18 healthy controls. The levels of NO₂-OA were found to be significantly higher in the plasma of patients (21.7 ± 9.8 nM) versus healthy controls (12.6 ± 6 nM) (p-value < 0.01). Whereas the levels of NO₂-LA were comparable in both groups (3 ± 1 nM in patients, 3.2 ± 1.7 nM in controls, p-value = 0.87288). The early elevation of NO₂-OA in plasma samples, which were collected 2–3 h post myocardial injury, implies the potential use of NO₂-OA levels as a biomarker for IHD after further investigation with a larger number of IHD patients. To our knowledge, this is the first comparative study on the levels of NO₂-FAs in humans with and without IHD. Full article

In this study, a fast, concise and reliable ultra-high performance liquid chromatography-fluorescence (UHPLC/FLD) detection method for simultaneous quantification of avermectins (AVMs), including avermectin (AVM), ivermectin (IVM), emamectin (EMM), moxidectin (MOX) and doramectin (DOR) in six aquatic foods was established. Based on the QuEChERS pretreatment method, the samples were extracted with 0.2% (v/v) ammonia acetonitrile. N-methyl imidazole mixed with acetonitrile (1:1, v/v) and trifluoroacetic anhydride with acetonitrile (1:2, v/v) were used as derivatization reagents. The mobile phase consists of acetonitrile and water with a flow rate of 1.0 mL/min. An Infinity Lab Poroshell 120 EC-C18 column was used for optimum chromatographic separation of target analytes at 40 °C; the excitation and emission wavelengths were set at 365 nm and 465 nm, respectively. In six kinds of aquatic foods, the limits of detection (LODs) of AVM, IVM, EMM, MOX, and DOR were 2.7 μg/kg, 1.8 μg/kg, 2.1 μg/kg, 1.2 μg/kg, and 2.7 μg/kg, respectively, and the limits of quantification (LOQs) of AVM, IVM, EMM, MOX, and DOR were 5 μg/kg, 4.5 μg/kg, 4.5 μg/kg, 3.5 μg/kg and 5.0 μg/kg, respectively. The recoveries were all above 85.38% when the samples were spiked with the target compounds at the concentration level of 5, 10, 50, and 100 μg/kg. The intra-day and inter-day relative standard deviations (RSDs) were all less than 15%. This method considers the requirements of sensitivity, accuracy, and economics of the instrument. Full article

The study of the urban context in the contemporary center of Portugal’s capital city uncovered traces of daily lives that were abruptly interrupted and utterly transformed by the Great Lisbon Earthquake on the morning of 1 November 1755. Charred organic residue was recovered from a cylindrical vessel excavated from the storage area of the town house at the Rossio square. The archaeological sample was studied through a multi-analytical approach based on microstructural, elemental and biomolecular characterization by attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FT-IR), variable pressure scanning electron microscopy coupled to energy dispersive X-ray spectroscopy (VP-SEM-EDS), and gas chromatography coupled with mass spectrometry (GC-MS). The residue was identified as human faeces collected in the ceramic vessel for disposal, and further analysis provided additional information about diet and the living conditions in the 18th century. Full article