Chemical characteristics and biological activity screening of Pistacia lentiscus mastic gum and leaves from Türkiye.

BACKGROUND: Mastic gum is a resin that is produced by Pistacia lentiscus. It has many traditional uses, dating from ancient times, such as the treatment of gastrointestinal disorders and as a food additive. In this study, the leaves and mastic gum of trees of different ages from Karaburun and the Cesme peninsula in Türkiye were examined chemically and biologically. Flavonoids, and phenolic and fatty acid components were evaluated by a liquid chromatography system coupled with high resolution mass spectrometry (LC-HRMS) and gas chromatography with flame ionization detection (GC-FID). Cytotoxicity was screened against several cancer and healthy cell lines using a 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl-2H-tetrazolium bromide (MTT) assay. Inducible nitric oxide synthase (iNOS) inhibition was determined on lipopolysaccharide (LPS)-induced murine macrophage cell line (RAW 264.7) cells. Antiviral activity was measured against avian coronavirus using an in ovo virucidal antiviral activity assay. RESULTS: The main phenolic constituents of the gum were found to be salicylic, rosmarinic, and caffeic acids whereas the most abundant compounds detected were flavonoids in the leaf extracts. The most abundant fatty acids in hexane extracts were palmitic and oleic acids. All gum extracts except 3-year-old gum had significant cytotoxic activity on HeLa (IC50 1.74 ± 0.03-4.76 ± 0.95) and PC-3 (0.64 ± 0.25-6.22 ± 1.40) cells. Moreover, reducing virus activity by fivefold or sixfold logarithmically between the range of 5-10 µg g-1 of 30-year-old gum extracts underscored the biological activity. CONCLUSION: In ovo antiviral activity studies on the P. lentiscus were conducted for the first time. The mastic gum and leaves obtained from P. lentiscus may have strong potential in terms of their chemical content and antiviral and cytotoxic activity. As a consequence of these properties, it is a sustainable, renewable natural resource that can be used as an additive and flavoring in the food and pharmaceutical industries. © 2023 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.

Chemical profile of the Anatolian Sideritis species with bioactivity studies.

CONTEXT: The genus Sideritis L. (Lamiaceae) is represented by 46 species in Turkey with an 79% endemism ratio, 42 of 46 belonging to the section Empodoclia. OBJECTIVE: In this review article, Sideritis species growing in Turkey have been evaluated for phytochemical constituents and biological activities. METHODS: The data for the isolates, components and extracts of the Anatolian Sideritis species and their bioactivity studies were retrieved from the main databases WoS, Scopus and PubMed from 1975 until 31 December 2022. RESULTS: In this review article, terpenoids, flavonoids, phenolics and other secondary metabolites isolated from Turkish Sideritis species were reported. Anatolian Sideritis species, which primarily consist of monoterpenes and sesquiterpenes, were studied in detail. Sideritis plants are represented by 46 species in Turkey, and 25 of them were investigated for their diterpenoids through isolation or LC-MS studies. Most of the diterpenoids of Turkish Sideritis species have ent-kaurene skeleton, among them linearol, siderol, 7-epicandicandiol and sideridiol were found to be the main compounds. Exceptionally, labdane, pimarane and beyerene diterpenoids were only found in a few species. For phenolics and flavonoids, only 12 species were investigated until now, and they were found to be rich in phenylethanoid glycosides and flavonoid glycosides. In terms of activity, most of the species were tested for antioxidant activity, followed by antimicrobial and anti-ulcer/anti-inflammatory activities. Their cytotoxic, enzyme inhibitory, antinociceptive and antistress activities were less frequently studied. CONCLUSIONS: Sideritis species should be considered promising therapeutic agents in the treatment of upper respiratory tract and ulcer/inflammatory diseases.

Antioxidant, Antiglaucoma, Anticholinergic, and Antidiabetic Effects of Kiwifruit (Actinidia deliciosa) Oil: Metabolite Profile Analysis Using LC-HR/MS, GC/MS and GC-FID.

Determining the antioxidant abilities and enzyme inhibition profiles of medicinally important plants and their oils is of great importance for a healthy life and the treatment of some common global diseases. Kiwifruit (Actinidia deliciosa) oil was examined and researched using several bioanalytical methods comprehensively for the first time in this research to determine its antioxidant, antiglaucoma, antidiabetic and anti-Alzheimer's capabilities. Additionally, the kiwifruit oil inhibitory effects on acetylcholinesterase (AChE), carbonic anhydrase II (CA II), and α-amylase, which are linked to a number of metabolic illnesses, were established. Furthermore, LC-HRMS analysis was used to assess the phenolic content of kiwifruit oil. It came to light that kiwifruit oil contained 26 different phenolic compounds. According to the LC-HRMS findings, kiwifruit oil is abundant in apigenin (74.24 mg/L oil), epigallocatechin (12.89 mg/L oil), caryophyllene oxide (12.89 mg/L oil), and luteolin (5.49 mg/L oil). In addition, GC-MS and GC-FID studies were used to ascertain the quantity and chemical composition of the essential oils contained in kiwifruit oil. Squalene (53.04%), linoleoyl chloride (20.28%), linoleic acid (2.67%), and palmitic acid (1.54%) were the most abundant compounds in kiwifruit oil. For radical scavenging activities of kiwifruit oil, 1,1-diphenyl-2-picryl-hydrazil (DPPH•) and 2,2'-azino-bis(3-ethylbenzthiazoline-6-sulfonic acid) (ABTS•+) radicals scavenging techniques were examined. These methods effectively demonstrated the potent radical scavenging properties of kiwifruit oil (IC50: 48.55 µg/mL for DPPH•, and IC50: 77.00 µg/mL for ABTS•+ scavenging). Also, for reducing capabilities, iron (Fe3+), copper (Cu2+), and Fe3+-2,4,6-tri(2-pyridyl)-S-triazine (TPTZ) reducing abilities were studied. Moreover, kiwifruit oil showed a considerable inhibition effect towards hCA II (IC50: 505.83 µg/mL), AChE (IC50: 12.80 µg/mL), and α-amylase (IC50: 421.02 µg/mL). The results revealed that the use of kiwifruit oil in a pharmaceutical procedure has very important effects due to its antioxidant, anti-Alzheimer, antidiabetic, and antiglaucoma effects.

Comprehensive Metabolite Profiling of Cinnamon (Cinnamomum zeylanicum) Leaf Oil Using LC-HR/MS, GC/MS, and GC-FID: Determination of Antiglaucoma, Antioxidant, Anticholinergic, and Antidiabetic Profiles.

In this study, for the first time, the antioxidant and antidiabetic properties of the essential oil from cinnamon (Cinnamomum zeylanicum) leaves were evaluated and investigated using various bioanalytical methods. In addition, the inhibitory effects of cinnamon oil on carbonic anhydrase II (hCA II), acetylcholinesterase (AChE), and α-amylase, which are associated with various metabolic diseases, were determined. Further, the phenolic contents of the essential oil were determined using LC-HRMS chromatography. Twenty-seven phenolic molecules were detected in cinnamon oil. Moreover, the amount and chemical profile of the essential oils present in cinnamon oil was determined using GC/MS and GC-FID analyses. (E)-cinnamaldehyde (72.98%), benzyl benzoate (4.01%), and trans-Cinnamyl acetate (3.36%) were the most common essential oils in cinnamon leaf oil. The radical scavenging activities of cinnamon oil were investigated using 1,1-diphenyl-2-picryl-hydrazil (DPPH•), 2,2'-azino-bis(3-ethylbenzthiazoline-6-sulfonic acid), and (ABTS•+) bioanalytical scavenging methods, which revealed its strong radical scavenging abilities (DPPH•, IC50: 4.78 µg/mL; and ABTS•+, IC50: 5.21 µg/mL). Similarly, the reducing capacities for iron (Fe3+), copper (Cu2+), and Fe3+-2,4,6-tri(2-pyridyl)-S-triazine (TPTZ) were investigated. Cinnamon oil also exhibited highly effective inhibition against hCA II (IC50: 243.24 µg/mL), AChE (IC50: 16.03 µg/mL), and α-amylase (IC50: 7.54µg/mL). This multidisciplinary study will be useful and pave the way for further studies for the determination of antioxidant properties and enzyme inhibition profiles of medically and industrially important plants and their oils.

Two new eudesmane-type sesquiterpene derivatives from Lecokia cretica (Lam.) DC.

Two new sesquiterpene glucosides, 1α,6ß,9ß-trihydroxy-eudesm-4(15)-en-1,6-O-ß-diglucopyranoside (1) and 1α,6ß,9ß-trihydroxy-eudesm-3-en-1,6-O-ß-diglucopyranoside (2) were obtained along with the 1α,6ß,9ß-trihydroxy-5,10-bis-epi-eudesm-3-en-6-O-ß-D-glucopyranoside (3), chlorogenic acid (4), luteolin 7-O-rutinoside (5) and luteolin 7-O- glucoside (6) from the whole plant parts of Lecokia cretica. Their structures were determined on the basis of 1 D, 2 D NMR and HRMS analyses. The in vitro cytotoxic activity of compounds 1-3 against human lung cancer cells (A549) and normal human lung cells (BEAS-2B) was determined using the MTT colorimetric assay. All the tested eudesmane derivatives were found to be inactive.

Polyphenol Contents, Potential Antioxidant, Anticholinergic and Antidiabetic Properties of Mountain Mint (Cyclotrichium leucotrichum).

In the present work, antioxidant and antidiabetic potentials of mountain mint [Cyclotrichium leu-cotrichum (Stapf ex Rech. Fil.) Leblebici] was the first time appraised. In this sense, methanol (MECL) and water (WECL) extracts were obtained from aerial parts of mountain mint (Cyclotrichium leucotrichum) and studied for their antioxidant ability by several bioanalytical assays. Also, their inhibition profiles were realized toward several metabolic enzymes connected to some diseases, including butyrylcholinesterase (BChE), α-glycosidase, acetylcholinesterase (AChE), and α-amylase enzymes. Additionally, their phenolic contents were determined by putative chromatographic method of LC/MS/MS. Consequently, nineteen phenolic molecules were identified in MECL and fifteen phenolic molecules were found in WECL. Also, antioxidant effects of both extracts were studied using by the methods of 1,1-diphenyl-2-picryl-hydrazyl (DPPH⋅), 2,2'-azinobis(3-ethylbenzthiazoline-6-sulfonic acid) (ABTS.+ ) and N,N-dimethyl-p-phenylenediamine (DMPD.+ ) scavenging activities, ferric (Fe3+ ) and cupric (Cu2+ ) ions and Fe3+ -2,4,6-tri(2-pyridyl)-s-triazine (TPTZ) reducing capacities. MECL and WECL were found as powerful DPPH⋅ (IC50 : 23.74 and 28.85 µg/mL), ABTS.+ (IC50 : 12.53 and 14.05 µg/mL) and DMPD.+ scavenging effects (IC50 : 43.52 and 54.80 µg/mL). Also, both extracts demonstrated the effective inhibition on AChE (IC50 : 69.31 and 115.51 µg/mL), BChE (IC50 : 57.75 and 86.62 µg/mL), α-glycosidase (IC50 : 36.47 and 62.94 µg/mL) and α-amylase (IC50 : 1.01 and 3.43 µg/mL). This study will be useful for future studies to determine the antioxidant properties and enzyme inhibition profile of food, medical and industrially important plants.

Antidiabetic, anticholinergic and antioxidant activities of aerial parts of shaggy bindweed (Convulvulus betonicifolia Miller subsp.) - profiling of phenolic compounds by LC-HRMS.

In order to evaluate the antioxidant activity of evaporated ethanolic extract (EESB) and lyophilized water extract (WESB) of Shaggy bindweed (Convulvulus betonicifolia Mill. Subs), some putative antioxidant methods such as DPPH· scavenging activity, ABTS•+ scavenging effect, ferric ions (Fe3+) reduction method, cupric ions (Cu2+) reducing capacity, and ferrous ions (Fe2+) binding activities were separately performed. Also, ascorbic acid, α-tocopherol and BHT were used as the standard compounds. Additionally, some phenolic compounds that responsible for antioxidant abilities of EESB and WESB were screened by liquid chromatography-high resolution mass spectrometry (LC-HRMS). At the same concentration, EESB and WESB demonstrated effective antioxidant abilities when compared to standards. In addition, EESB demonstrated IC50 values of 1.946 µg/mL against acetylcholinesterase (AChE), 0.815 µg/mL against α-glycosidase and 0.675 µg/mL against α-amylase enzymes.

Identification of natural compounds of Jurinea species by LC-HRMS and GC-FID and their bioactivities.

The Jurinea Cass. is one of the most important genera within Asteraceae and it comprises about 250 species in total. This genus is known for its numerous biological activities such as antioxidant, antimicrobial, antilipid peroxidation, anticholinesterase, antileishmanial activities. The aim of this study was to determine chemical composition and biological activities of ethanol and n-hexane extracts of three different Jurinea species. For this purpose, different parts of J. mollis, J. cadmea and J. pontica were extracted and totally six n-hexane and six ethanol extracts were obtained. Fatty acid content of n-hexane extracts was determined by GC-FID whereas phenolic and flavonoid content of ethanol extracts by LC-HRMS. Palmitic acid (16:0) was detected as the most abundant fatty acid in all n-hexane extracts with the rates ranging from 42.16%-55.08%, except flowers of J. mollis (JMF) and J. cadmea (JCF). LC-HRMS analysis showed the rutin content of all extracts was higher than other flavonoids, except of J. cadmea flowers, whereas apigenin-7-glucoside was found the most abundant in JCF. Cytotoxic effects of the extracts on HeLa and HEK-293 cells were determined by MTT method, and antioxidant activities were evaluated by DPPH and CUPRAC assays. Ethanol extract of J. mollis flowers significantly inhibited cancerous HeLa cells, with the IC50 value of 9.683 µg/mL while it was more less toxic on healthy HEK-293 cells. Ethanol extracts of J. mollis flowers and J. mollis steams-leaves (JMSL) showed the highest antioxidant activity by a DPPH inhibition % of 45.516 ± 2.497 and 56.671 ± 1.496, respectively. JMF and JMSL have also the highest CUPRAC values (0.880 ± 0.067 and 1.085 ± 0.152 mmol TR/g DWE, respectively). Total flavonoid content was determined using aluminum chloride colorimetric assay while total tannin and phenolic content by Folin Chiocalteu's reagent. Results showed that JMSL has the highest total phenolic (108.359 ± 6.241 mg GAE/ G DWE) and flavonoid (32.080 ± 4.385 mg QE/ g DWE) contents whereas JMF has the highest tannin content (121.333 ± 17.889 mg TAE/ g DWE). In the light of these results, various parts of Jurinea species may be regarded as alternative sources for cytotoxic and/or antioxidant flavonoids, phenolics and unsaturated fatty acids that can arouse the interest of pharmaceutical, food and cosmetic industries.

Composition of the essential oil of Satureja metastasiantha: a new species for the flora of Turkey.

The aerial parts of Satureja metastasiantha were hydrodistilled for 3 h using a Clevenger-type apparatus. The essential oils were analyzed by gas chromatography/flame ionization detector and gas chromatography/mass spectrometry, simultaneously, the main compounds of which were characterized as p-cymene (22.3%), thymol (21.0%), carvacrol (18.4%), and γ-terpinene (12.1%). Antioxidant capacity, acetylcholinesterase and butyrylcholinesterase inhibition effects, and antimicrobial and antifungal properties of the species were evaluated. The anticholinesterase activity of the essential oil of S. metastasiantha was observed with 30% inhibition at 200 µg/mL. The essential oil of the species showed activity against Staphylococcus aureus with 128 µg/mL minimum inhibitory concentration value.

Phytochemical content, antioxidant activity, and enzyme inhibition effect of Salvia eriophora Boiss. & Kotschy against acetylcholinesterase, α-amylase, butyrylcholinesterase, and α-glycosidase enzymes.

Many taxa of Salvia genus have been used in herbal beverages, food flavoring, cosmetics, and pharmaceutical industry. In this paper, chemical compounds of Salvia eriophora (S. eriophora) leaves were determined by LC-MS/MS (Liquid Chromatography tandem Mass Spectrometry). Salvigenin (158.64 ± 10.8 mg/kg), fumaric acid (123.09 ± 8.54 mg/kg), and quercetagetin-3.6-dimethylether (37.85 ± 7.09 mg/kg) were detected as major compounds in the ethanol extract, whereas fumaric acid (555.96 ± 38.56 mg/kg), caffeic acid (103.62 ± 20.51 mg/kg), and epicatechin (83.19 ± 8.43 mg/kg) were detected as major compounds in the water extract. Furthermore, enzyme inhibition of S. eriophora against acetylcholinesterase (AChE), α-amylase (AM), butyrylcholinesterase (BChE), and α-glycosidase (AG) enzymes were detected. AChE, BChE, AG, and AM enzymes were very strongly inhibited by S. eriophora water extract (WES) and S. eriophora methanol extract (MES). Additionally, antioxidant potential of S. eriophora was determined by in vitro analytical methods. IC50 values of WES and MES were performed for radicals. PRACTICAL APPLICATIONS: Metabolic enzymes have crucial functions on living systems due to inhibition or activation of them mainly attributed with some health disorders. AChE, BChE, AM, and AG enzymes have important roles on carbohydrate metabolism or cholinergic pathways. The relation between enzyme inhibition effect and phenolic compounds or antioxidant activity need to be confirmed. Thus, many studies tested to clarify this relation for pure samples or plant extracts. To the best of our knowledge, this is the first report about inhibition effects of Salvia eriophora extracts against AChE, BChE, AM, and AG enzymes as well as their phenolic contents and antioxidant activities.

Simultaneous determination of several flavonoids and phenolic compounds in nineteen different Cephalaria species by HPLC-MS/MS.

Cephalaria species in Turkey known as "Pelemir" and they have many different biological activities due to their wide range of chemical content. The main goal of this study is determine the flavonoids and phenolic acids in Cephalaria species using high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). This method was developed for quantitation of reported compounds using reverse phase Fortis C18 (150 × 3 mm × 5 µm) column with a gradient of 0.1% formic acid solution (A) in water and (B) in methanol in ESI mode. The recoveries of developed method were obtained in the range of 90.4-109.4%. Limit of detection (LOD) and limit of quantification (LOQ) values were calculated in the range of 0.3-25.2 ppb and 3.0-102.3 ppb for the reported compounds. Uncertainty evaluations of all compounds were reported. Twenty-five flavonoids, five simple phenolics, two triterpenoids, one iridoid and vitamin C successfully identified and quantified for nineteen Cephalaria species. The main flavonoids in the studied species were determined as cyanidin-3-O-glucoside, luteolin-7-O-glucoside, kaempherol-3-O-glucoside, hyperoside, hesperidin, luteolin and quercetin while salicylic and caffeic acids were detected as major phenolic acids in the analyzed samples. This is the first full characterization study for nineteen Cephalaria species via HPLC-MS/MS.

Phenolic compounds from the aerial parts of Clematis viticella L. and their in vitro anti-inflammatory activities.

Phytochemical investigations on the EtOH extract of Clematis viticella led to the isolation of six flavonoid glycosides, isoorientin (1), isoorientin 3'-O-methyl ether (2), quercetin 7-O-α-L-rhamnopyranoside (3), quercetin 3,7-di-O-α-L-rhamnopyranoside (4), manghaslin (5) and chrysoeriol 7-O-ß-D-glucopyranoside (6), one phenylethanol derivative, hydroxytyrosol (7), along with three phenolic acids, caffeic acid (8), (E)-p-coumaric acid (9) and p-hydroxybenzoic acid (10). The structures of the isolates were elucidated on the basis of NMR and HR-MS data. All compounds were isolated from C. viticella for the first time. Compounds 7 and 8 showed significant anti-inflammatory activity at 100 µM by reducing the release of NO in LPS-stimulated macrophages comparable to positive control indomethacin. Compounds 3 and 7 exhibited anti-inflammatory activity through lowering the levels of TNF-α while 1, 3 and 5 decreased the levels of neopterin better than the positive controls.

Different propolis samples, phenolic content, and breast cancer cell lines: Variable cytotoxicity ranging from ineffective to potent.

Researchers have started focusing on investigating the anticarcinogenic effects of natural products with the slightest side effects possible, because current breast cancer treatment approaches are unable to achieve absolute success especially on aggressive subtypes. Propolis is among these products with its antimicrobial, antifungal, anti-inflammatory, and anticancer effects. Therefore, seven different samples were collected from different regions (Argentina, China, and Istanbul-Turkey) and applied on nonaggressive breast cancer cell line (BCCL) MCF-7 and aggressive cell lines SK-BR-3, and MDA-MB-231. Initially, the phenolic/flavonoid constituents of the propolis ethanol extracts were investigated by liquid chromatography-mass spectrometry-mass spectrometry (LS-MS/MS) and high-performance liquid chromatography (HPLC) analyses. Then, the anticarcinogenic effects of the propolis samples on MCF-7, SK-BR-3, MDA-MB-231 were evaluated by WST1 analysis and only selected ones on MCF-10A and hPdLF. According to the LS-MS/MS and HPLC analysis, Turkey originated propolis (Turkey3) were found to be richer than the other propolis samples in terms of phenolic/flavonoid compounds. Turkey propolis significantly inhibited cell proliferation in both nonaggressive and aggressive BCCL (P < 0.01). Therefore, Turkey3 propolis was selected for further evaluation using Annexin V-PI apoptosis detection assays. In addition, selected compounds among the propolis contents such as galangin, caffeic acid, apigenin, quercetin, and ferulic acid were applied to the MCF-7 cell line to detect cytotoxic and apoptotic effects. Galangin, caffeic acid, apigenin, and quercetin remarkably induced cell proliferation inhibition at all time intervals, whereas ferulic acid was found non efficient on the MCF-7 cell line. Annexin V-PI assay clarified that all cell proliferation inhibitions were markedly apoptotic. Our findings indicated that the inhibition effect of propolis on breast cancer cell proliferation was in a propolis type-, dose- and time-dependent fashion. Turkey3 propolis showed statistically significant cytotoxic effects on both the nonaggressive and aggressive BCCL. These findings were consistent with the effects of its rich phenolic and flavonoid contents, in terms of variety. © 2018 IUBMB Life, 71(5):619-631, 2019.

Oligomer based real-time detection of microorganisms producing nuclease enzymes.

In this study, we provide a method using fluorescently labeled oligonucleotides for the diagnosis of microorganisms producing nucleases in real time, while growing them in culture media. The detection of such microorganisms was possible in a short period of time, as short as 10 minutes up to a maximum of 8 hours, depending on the bacterial density. We also showed the suitability of this new method for determination of minimum inhibitory concentration (MIC) in culture media in a very short period of time, compared to conventional methods. We believe that it can make a significant contribution to gain new insights for analysis of complex materials such as clinical samples, food samples and environmental samples.

Screening of Hallucinogenic Compounds and Genomic Characterisation of 40 Anatolian Salvia Species.

INTRODUCTION: Salvia, an important and widely available member of Lamiaceae family. Although comparative analysis on secondary metabolites in several Salvia species from Turkey has been reported, their hallucinogenic chemicals have not been screened thoroughly. OBJECTIVE: This study provides LC-MS/MS analysis of 40 Salvia species for screening their psychoactive constituents of salvinorin A and salvinorin B. 5S-rRNA gene non-coding region of Salvia plants was sequenced, aligned and compared with that sequence of Salvia divinorum plant. METHODOLOGY: Targeted molecules of salvinorin A and salvinorin B were quantified, using LC-MS/MS, from all aerial parts of 40 Salvia species, collected from different parts of Turkey. Regions of 5S-rRNA gene from different species were amplified by polymerase chain reaction and DNA sequences were aligned with Salvia divinorum DNA sequences. RESULTS: Very few of the Salvia species (S. recognita, S. cryptantha and S. glutinosa) contained relatively high levels of salvinorin A (212.86 ± 20.46 µg/g, 51.50 ± 4.95 µg/g and 38.92 ± 3.74 µg/g, respectively). Salvinorin B was also found in Salvia species of S. potentillifolia, S. adenocaulon and S. cryptantha as 2351.99 ± 232.22 µg/g, 768.78 ± 75.90 µg/g and 402.24 ± 39.71 µg/g, respectively. The sequences of 5S-rRNA gene of 40 different Salvia species were presented and it was found that none of the Salvia species in Turkey had similar DNA sequence to Salvia divinorum plant. CONCLUSION: This is the first report of screening 40 Salvia species in Turkey according to their psychoactive constituents, salvinorin A and salvinorin B and their genomic structures. It is possible that some of these Salvia species may exhibit some psycho activity. Thus, they need to be screened further. Copyright © 2017 John Wiley & Sons, Ltd.

Syntheses and evaluation of multicaulin and miltirone-like compounds as antituberculosis agents.

Four multicaulin and miltirone-like phenanthrene derivatives were synthesised and evaluated as antituberculosis agents. The crucial step of the synthesis was Pschorr coupling of 4-(3-isopropyl-4-methoxyphenyl)-2-(2-aminophenyl)ethane (13) to give 2-isopropyl-3-methoxy-9,10-dihydrophenanthrene (9) and 4-isopropyl-3-methoxy-9,10-dihydrophenanthrene (9a). Compound 9 was converted to multicaulin and miltirone-like phenanthrene derivatives by further reactions. The best antituberculosis activity was exhibited by 2-isopropylphenanthrene-3-ol (11).

Determination of neurotoxic agents as markers of common vetch adulteration in lentil by LC-MS/MS.

Vicia sativa (common vetch), which contains ß-cyanoalanine (BCA) and γ-glutamyl ß-cyanoalanine (γGBCA) is used for adulteration of lentil and have neuro toxic effects on people and animals. Therefore the determination of BCA and γGBCA analytes in accurate and reliable manner has high importance for human and animal health. LC-IDMS/MS method has been developed and validated for quantitative analyses of ß-cyanoalanine and 13C labeled BCA is used as an internal standard in γGBCA analysis. In order to validate the method, linearity, recovery, precision (repeatability), intermediate precision, limit of detection, and limit of quantification parameters were investigated. The correlation coefficient was found to be greater than 0.99 for both analytes. The recoveriess were determined as 95.8% for BCA and 97.4% for γGBCA. The relative expanded measurement uncertainties of ß-cyanoalanine and γ-glutamyl-ß-cyanoalanine were obtained as 4.6% and 5.8%, respectively with the coverage factor, k, is 2 and at 95% confidence level.

A class of sulfonamides as carbonic anhydrase I and II inhibitors.

Four groups of novel sulfonamide derivatives: (i) acetoxybenzamide, (ii) triacetoxybenzamide, (iii) hydroxybenzamide and (iv) trihydroxybenzamide, all having thiazole, pyrimidine, pyridine, isoxazole and thiadiazole moieties were prepared and their inhibitory effects were studied on two metalloenzymes, i.e. carbonic anhydrase isozymes (hCA I and II), purified from human erythrocyte cells by Sepharose-4B-l-tyrosine-sulfanilamide affinity chromatography. These enzymes are present in almost all living organisms to catalyse the synthesis of bicarbonate ion (HCO3-) from carbon dioxide and water. The sulfonamide derivatives were found to be active against hCA I and II in the range of 2.62-136.54 and 5.74-210.58 nM, respectively.

Potential reference measurement procedures for PBDE in surface water at levels required by the EU Water Frame Directive.

Polybrominated diphenylethers (PBDE), used as flame retardants, are named as priority substances in the Directive 2000/60/EC of the European parliament and of the council establishing a framework for Community action in the field of water policy. An annual average environmental quality standard (EQS) for inland surface waters of 0.0005 µg/L (0.0002 µg/L for other surface waters) for PBDE congeners involved in the technical penta-PBDE mixtures containing PBDE with five bromine atoms has been established. The directives focus especially on the congeners PBDE 28, 47, 99, 100, 153 and 154 contained in the penta-PBDE mixture. Up to now, no reference measurement procedures have been established reaching the limits of quantification (LOQs) and the associated uncertainties as defined in the directives with results traceable to the SI. Within a recent European project on metrology, different approaches for the traceable quantification of PBDE, based on liquid/liquid or solid phase extraction followed by the detection with gas chromatography coupled to either inductively coupled plasma mass spectrometry or triple quadrupole mass spectrometry, were investigated and the related LOQs and expanded uncertainties of the results were compared. A complete uncertainty budget for each method was estimated according to the Guide to the Expression of Uncertainty in Measurement (GUM). All presented analytical procedures can serve as reference measurement procedures regarding the LOQs and their associated expanded uncertainties for monitoring the six priority PBDEs named above. LOQs as low as 0.026 ng/kg with an associated expanded uncertainty of 0.002 ng/kg could be achieved.