In this study, a gas chromatography-tandem mass spectrometry (GC-MS/MS) instrument, which has been widely used in recent years and has high separation power, selectivity and ability to identify pesticides has been used. It is aimed that the main criterion of this analytical method, in which the QuEChERS methodology is used, is applicable to fast, easy, cheap, environmentally friendly and different matrices. At the same time with this method, 123 pesticide residues and their degradation products were quantitatively assayed by GC-MS/MS as well as method validations in tomatoe, lemon, lettuce, almonds, raisins, honey, green pepper, milk and flour. Tomatoe was selected as potential reference matrixes for the target. The steps of concentration and solvent exchange were performed in the resultant extracts for the purpose of improving analytical performance in terms of recovery, precision, linearity, of reducing the amount of co-extracts. Multiple reaction monitoring (MRM) was used to identify and quantify the pesticides. The samples were extracted with 1% acetic acid in acetonitrile, anhydrous magnesium acetate, anhydrous magnesium sulfate and clearing agent. For all pesticides, good linear calibrations with coefficients (R2) ≥0.99 for nearly all of the analytes were obtained. Limit of quantitation of most of the pesticides were in the range of 5-10 ng/g, and recovery of the method validation accuracy parameter was done at two different concentrations 10 ng/g and 50 ng/g were 88.6 - 99.7% and CV 1.60 – 14.0%.
In this study, the compositions of Calvatia gigantea were first analyzed in order to elucidate its chemical basis for development as a health-enhancing food or medicine. This study investigates the chemical composition (nutritional value; phenolic, sugar and fatty acid content; aroma compounds) and antioxidant properties (radical scavenging activity, reducing power, and inhibition of lipid peroxidation) of C. gigantea. The results showed that C. gigantea contains phenolic compounds and sugars and is rich in polyunsaturated fatty acids (67.93%), proteins (34.37%), and carbohydrates (51.97%). The most abundant compounds were gentisic acid (23.26 µg/g; as a phenolic compound), trehalose (9.78 g/100g; as a sugar), and hexanal (34.71%; as an aroma compound). These findings suggest that C. gigantea might be a promising source of medicine and has the potential to be a health food and food supplementary product.
An accurate, reliable and fast multianalyte/multiclass ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed and validated for the simultaneous analysis of 23 pharmaceuticals, belonging to different classes amphenicols, sulfonamides, tetracyclines, in honey samples. The method developed consists of ultrasonic extraction followed by UPLC–ESI–MS/MS with electrospray ionization in both positive mode and negative mode. The influence of the extraction solvents and mobile phase composition on the sensitivity of the method, and the optimum conditions for sample weight and extraction temperature in terms of analyte recovery were extensively studied. The identification of antibiotics is fulfilled by simultaneous use of chromatographic separation using an Acquity BEH C18 (100 mm x 2.1 mm, 1.7 µm) analytical column with a gradient elution of mobile phases and tandem mass spectrometry with an electrospray ionization. Finally, the method developed was applied to the determination of target analytes in honey samples obtained from the local markets and several beekeepers in Mugla, Turkey. Ultrasonic-extraction of pharmaceuticals from honey samples is a well-established technique by UPLC–ESI–MS/MS, the uniqueness of this study lies in the simultaneous determination of a remarkable number of compounds belonging to 23 drug at the sub-nanogram per kilogram level.
Wild edible and medicinal mushroom, Calvatia gigantea, was quantitatively analyzed for the determination of its free amino acids using ultra performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS). The concentrations of total free amino acids, essential and non-essential amino acids were 199.65mg/100g, 113.69mg/100g, and 85.96mg/100g in C. gigantea, respectively. This study showed that C. gigantea, so called a giant puffball mushroom, has free amino acids content. The essential amino acids: tryptophan, isoleucine, valine, phenylalanine, leucine, threonine, lysine, histidine, methionine, and the non-essential amino acids: tyrosine, 4-hyrdroxy proline, arginine, proline, glycine, serine, alanine, glutamine, glutamic acid, aspargine, aspartic acid were detected.
The antioxidant activity of extracts of Armillaria tabescens , Leucopaxillus gentianeus and Suillus granulatus were determined for the first time by using five complementary tests; namely, β-carotene-linoleic acid, DPPH • scavenging, ABTS • + scavenging, metal chelating and CUPRAC assays. In DPPH • scavenging, ABTS•+ scavenging and CUPRAC assays, the ethylacetate extract of S. granulatus showed the best activity 91.52±0.97%, 89.67±0.15% and 3.90±0.09 at 400 μg mL -1 concentration, respectively while in β-carotene-linoleic acid assay, the methanol extract of this mushroom exhibited higher activity. In addition, among the extracts of mushroom species, particularly the hexane extracts showed better activity in metal chelating activity. The hexane extract of L. gentianeus exhibited the highest metal chelating activity (70.68±0.34%) at 400 μg mL -1 concentration. In conclusion, the results showed the antioxidant importance of the studied mushroom species, growing naturally in Anatolia. Thus, particularly S. granulatus may have been helped people to protect against lipid peroxidation and free radical damage, and its extracts will probably use for the development of safe food products and additives.
Hydroxymethylfurfural (HMF) veya 5-(Hydroxymethyl)furfural, 5-hydroxymethyl-2furancarbaldehyde ekerin dehidrasyonu sonucu olu an organik bir bile iktir. Bu molekül aldehit ve alkol i levsel gruplar içeren bir furan türevi olup suda oldukça iyi çözünür. HMF, uht-süt, meyve suyu, bal gibi s l i lem görmü birçok g dada tespit edilmi tir. Asl nda HMF taze g dalarda bulunmaz ancak kurutma veya pi irme gibi s l i lemler s ras nda eker içeren g dalarda do al olarak olu ur. HMF Maillard tepkimesine ve karamelizasyon esnas nda olu ur. Bu g dalarda depolama s ras nda da yava bir ekilde olu ur. Asidik artlar HMF olu umunu tetikler [1]. HMF a r s l i lemin göstergesidir. Bal n s t lmad n n garanti alt na al nmas için codex alimentarius standard nda bal n HMF limitini 40 mg/kg’dan az, tropik ballarda ise 80 mg/kg’dan az olmas gerekti ini belirtilmektedir. Taze bal pH de eri, s cakl k ve üretim tarihine ba l olarak 15 mg/kg’dan az HMF de erine sahiptir. Bu çal mada ileri sürdü ümüz metot, HMF (5-hydroxymethyl-2-furancarbaldehyde) miktar tayini yapmak üzere tüm bal numunelerine uygulanabilir. Baldan elde edilen HMF de eri, mg HMF / 1 kg bal olarak verilir. Baldaki HMF s v kromatografi yöntemi ile ayr larak, UV dedektörü yard m yla kantitatif analizlerinin yap lmas prensibine dayan r. Pikler tutunma zamanlar na göre tan mlan r. Hesaplama external standard n pik yüksekli i veya pik alan na göre yap l r. Bu metot Jeuring ve Kuppers’in çal malar na dayanmaktad r [2]. Bal’da HMF (5-hydroxymethyl-2-furancarbaldehyde) tayini ve metot geli tirme i lemleri HPCL/DAD cihaz kullan larak yap lm olup, numune matriksi olarak piyasadan temin edilen “Çiçek Bal ” seçilmi tir. Deneysel çal malarda yüksek konsantrasyon kademesi 100 mg/kg, orta konsantrasyon kademesi 40 mg/kg, dü ük konsantrasyon kademesi olarak 5 mg/kg seçilmi tir. Seçicilik, ölçülmesi hedeflenen bile i in analiz edilece i matrikste do ru olarak tespit edilmesidir. Seçicili i tespit etmek için HMF içermeyen blank bal numuneleri HPLC-diode array dedektöre enjekte edilmi ve her defas nda bu kromatogramlar kalibrasyon e risini olu turmakta kullan lan standart maddelerle kar la t r lm t r. HMF’nin al konma zaman nda (retention time) blank numunede hiçbir giri im (interferans) tespit edilmemi tir [3]. Hesaplama yapmak için HPLC bilgisayar yaz l m kullan larak, referans malzeme çözeltilerinden elde edilen verilerden kalibrasyon e risi çizildi. Elde edilen kalibrasyon e risi, numune tart m , seyreltme faktörü cihaz yaz l m taraf ndan hesaplamada kullan ld ve veriler elde edildi. Eski klasik metotlardan, White metoduna [4] göre HMF’nin sodium bisulphite’in varl nda ve yoklu undaki indirgenmesi bir spektrofotometre ile tespit edilirdi (AOAC 980.23) [5]. Winklerin fotometrik methodu [6] ise p-toluidine ve barbituric asit kullan lan bir renk tepkimesidir. Spektrofotometrik test genel ve belirsiz olabilir, çünkü HPLC ölçümlerinden daha yüksek sonuç ç kmas na neden olan maddeleri de tespit edebilmektedir. Ayr ca spektrofotometrik yöntemde kullan lan p-toluidine oldukça toksik ve kanserojendir.
Serratula L. (Astareceae) rich in ecdysteroid, phytoecdysteroids and flavonoids some have various biological activities including antibacterial and antitumor. The fatty acid profiles of four Serratula species were investigated by using GC and GC-MS techniques. Palmitic, oleic, linoleic and linolenic acids were found to be the main fatty acids. The unsaturation percentage was between 27.24-50.47%. The antioxidant activity of the extracts was determined by using four complementary tests; namely, beta-carotene-linoleic acid, DPPH center dot scavenging, CUPRAC and ferrous-ions chelating assays. The methanol extract of S. lasiocephala showed the highest activity in beta-carotene-linoleic acid, DPPH center dot scavenging and CUPRAC assays, while the hexane extract of S. radiata exhibited the best metal chelating activity. In addition, total phenolic and total flavonoid contents in the extracts were determined as pyrocatechol and quercetin equivalents, respectively. The in vitro anticholinesterase activity of extracts were tested against acetylcholinesterase (AChE) and butyrylcholinesterase (BChE) which are the key enzymes taking place in pathogenesis of Alzheimer's disease. Besides, the extracts were tested in vitro against tyrosinase enzyme which is associated with melanin hyperpigmentation. Except the hexane extracts of S. radiata and S. lasiocephala, the extracts showed moderate inhibition against AChE and BChE, while the only hexane extract of S. erucifolia and methanol extract of S. radiata exhibited tyrosinase inhibitory activity.
In this study, phenolic content of Pinus brutia's bark was examined using an ultra-performance liquid chromatography tandem mass spectrometry with electrospray ionization source (UPLC-ESI-MS/MS) working in multiple reaction monitoring mode. Ultrasonic extraction method with 50% ethanol solution was used for the extraction of bark. The bark of Pinus brutia consisted of 15 compounds: gallic acid, gentisic acid, protocatechuic acid, 4-hydroxy benzoic acid, catechin hydrate, vanillic acid, caffeic acid, vanillin, p-coumaric acid, ferulic acid, myricetin, resveratrol, luteolin, naringenin, kaempferol. Major compound detected was catechin hydrate (28.305 mg 100 g(-1) extract). The phenolic compounds of Pinus brutia extract and pycnogenol were compared, and it is shown that both of them consisted of considerable amount of phenolic compounds.
Mantarların yağ asit bileşimlerinin belirlenmesi, mantarın besinsel özelliklerinin açığa çıkarılmasına katkı sağlamaktadır. Mantarların yağ oranları düşük olmasına karşın polidoymamış yağ asitlerinin oranı yüksektir. Mantarlarda genel olarak, C12-C20 arasındaki normal yağ asitleri [1,2] ve C16-C24 hidroksi grup taşıyan yağ asitleri bulunmaktadır [1]. Mantar yağ asiti bileşimlerinde oleik, linoleik, ve palmitik asit majör bileşenler olarak bulunmaktadır[3]. Bu güne kadar yağ asitleri araştırılan bütün mantarlarda linoleik ve linolenik asit’in varlığı ortaya konulmuştur. Bu doymamış yağ asitleri insanların beslenmesinde önemli iki bileşendir. Özellikle uzun zincirli polidoymamış yağ asitleri insan sağlığı üzerinde faydalı etkilere sahip olduğu rapor edilmiştir [4].
Chemical composition of Chroogomphus rutilus, the edible mushroom species, was analyzed by using gas chromatography (GC), gas chromatography mass spectrometry (GC-MSD) and inductively coupled plasma mass spectrometry (ICP-MS). The silylated extract affords 19 components. Xylitol (56.28 %), glucitol (11.08 %), fumaric acid (10.92 %) and mannitol (6.79 %) were identified as the major compounds. The methylated extract possessed 13 fatty acids, and linoleic acid (41.61 %) and oleic acid (35.87 %) were the majors. In addition, the mineral and the heavy metal contents were tested for nine minerals and 12 heavy metals by using ICP-MS. In addition, the extracts were evaluated for cholinesterase inhibitory effects against acetyl-cholinesterase and butyrylcholinesterase which are the chief enzymes of Alzheimer’s disease. The antioxidative effect of the extracts was also determined by using five complimentary assays. Moreover, the hexane extract (IC50, 2.22 ± 0.13 μg/ml) and the ethyl acetate extract (IC50, 2.28 ± 0.18 μg/ml) exhibited a good lipid peroxidation inhibitory activity while the methanol extract demonstrated good butyrylcholinesterase inhibitory activity (IC50, 45.5 ± 1.1 μg/ml). In addition, total phenol and flavonoid contents of the extracts were also determined as pyrocatechol and quercetin equivalents, respectively. Because of its high antioxidant activity, C. rutilus might protect people against lipid peroxidation and free radical damage when consumed. It can be also used in food industry as preservative agents or extension of the shelf-life of foods. Since methanol extract indicated remarkable inhibitory activity being close to that of galantamine, it may be also useful as moderate cholinesterase inhibitory agents, particularly against butyrylcholinesterase.
The essential oil from the aerial parts of Salvia chrysophylla Staph (Lamiaceae), endemic to Turkey, was investigated by using GC and GC-MS. Fifty-four of 55 components, represented 99.52% of the total oil, were identified. The major components of the essential oil were found to be alpha-terpinenyl acetate (36.31%), beta-caryophyllene (15.29%), linalool (8.12%) and beta-elemene (4.26%). The antioxidant activity of the oil was investigated by using 2,2-diphenyl-1-picrylhydrazyl (DPPH) and beta-carotene/linoleic acid tests. Anticholinesterase activity was screened against acetylcholinesterase and butyrylcholinesterase which are the chief enzymes of Alzheimer's disease. The essential oil showed weak antioxidant activity. However, at 1 mg/mL concentration, the essential oil exhibited mild acetylcholinesterase (52.5+/-2.0%) and moderate butyrylcholinesterase (76.5+/-2.7%) inhibitory activity
The purpose of the present study is to investigate the effects of multiple-intelligence theory on students' achievement, attitude and retention. The study employed quasi-experimental design. The study was carried out with fifth grade students from Ataturk Primary School in Koyce?iz, Mu?la in 2004-2005 school year. The participants were divided into two groups as control and experimental groups. Traditional way of teaching was employed in the control group and multiple-intelligence-based teaching was used in the experimental group. The data obtained were analyzed through dependent and independent-samples t-test. The findings revealed that there are significant differences between the achievement, attitude, and retention of the experimental group and control group favoring the experimental group students exposed to multiple-intelligence based teaching.
Bu caly?manyn amacy, Coklu Zekâ Kuramy'na dayaly o?retimin o?rencilerin eri?i, tutum ve kalycylyk duzeyleri uzerine olan etkilerini ara?tyrmaktyr. Ara?tyrmada yary deneysel desen kullanylmy?tyr. Caly?ma, 2004-2005 e?itim-o?retim yyly guz doneminde Mu?la ili Koyce?iz ilcesindeki Pansiyonlu Ataturk Ylko?retim Okulu be?inci synyf o?rencilerinden iki grup uzerinde yurutulmu?tur. Kontrol grubunda geleneksel o?retim yontemi, deney grubunda Coklu Zekâ Kuramy'na dayaly o?retim yontemi uygulanmy?tyr. Verilerin analizi, ba?ymly ve ba?ymsyz gruplar t testi ile cozumlenmi?tir. Elde edilen bulgular, Coklu Zekâ Kuramy'na dayaly o?retim yonteminin uygulandy?y deney grubu ile geleneksel o?retim yonteminin uygulandy?y kontrol grubu o?rencilerinin ba?ary, tutum ve kalycylyk duzeyleri arasynda deney grubu lehine anlamly fark oldu?unu gostermi?tir.
The essential oil and methyl ester of hexane extract of Salvia chionantha Boiss. were analysed by GC and GC–MS. Totally, 54 components were detected in the essential oil and all of them were fully determined. Germacrene D (25.03%), β-caryophyllene (8.71%), spathulenol (5.86%) and α-humulene (4.82%) were identified as the major compounds. In the methylated hexane extract, 3-hydroxy hexadecanoic acid (39.39%), 3-hydroxy tetradecanoic acid (12.66%) and palmitic acid (12.02%) were the major fatty acids elucidated. The antioxidant activity of the essential oil and the hexane extract was determined by using four complementary test systems; namely, β-carotene-linoleic acid, DPPH scavenging, ABTS+ scavenging, and CUPRAC assays. In β-carotene-linoleic acid assay, the extract showed 81.2±0.1% lipid peroxidation inhibition at 0.8mg/mL concentration, while in ABTS+ assay the essential oil exhibited 77.4±0.5% inhibition at same concentration. Since, acetylcholinesterase and butyrylcholinesterase enzymes are taking place in pathogenesis of Alzheimer’s disease, in vitro anticholinesterase activity of the essential oil and the extract was also studied spectrophotometrically. At 0.5mg/mL concentration, the essential oil showed moderate acetylcholinesterase (56.7±1.9%) and butyrylcholinesterase (41.7±2.9%) inhibitory activity, while the extract was only exhibited activity (63.1±0.8%) against butyrylcholinesterase enzyme. Hence, the essential oil may be useful as a moderate anticholinesterase agent, particularly against acetylcholinesterase.
A novel spectrophotometric method to determine the amount of rosmarinic acid in unpurified methanol extracts of the plants was developed. Rosmarinic acid is a naturally occurring bioactive compound in plants as an ester of caffeic acid with 3,4-dihydroxyphenyl lactic acid. The developed method was based on the complexation of rosmarinic acid with Zr4+ ions, giving a maximum absorbance at 362nm. The absorptivity coefficient at this wavelength was found to be ε362=2.66×104Lmol−1cm−1. In fact, this method is also specified giving two more absorption bands in UV region at 299.5 and 263.5nm besides 362nm. In addition, the accuracy and sensitivity of the new developed method are compared with the direct UV and rosmarinic acid–Fe2+ complex spectrophotometric methods by using methanol extracts of 11 Salvia species. As a conclusion, the present method is faster, cheaper, and more selective than the conventional methods for rosmarinic acid.
In this study, essential oil compounds from the aerial parts of Coridothymus capitatus (L.) Reichb. were analysed by GC and GC/MS system, and total 28 constituents were identified. The main components were characterized as carvacrol (76,59%), alpha-phellandrene (6,04%), 1-octen-3-ol (5,13%), beta-caryophyllene (3,95%) and gamma-terpinene (1,72%). In addition, the antioxidant properties of essential oil and water and ethanol extracts from C. capitatus were examined. The antioxidant activity was investigated with three different methods: the beta-carotene bleaching test, the 2,2'-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging method and the total phenolic content. The total antioxidant activity measured by the beta-carotene bleaching test was highest in C. capitatus water extract (95,7%) while the free radical scavenging activity was highest in the plant's ethanol extract (90,7%). The amount of phenolic compounds in C. capitatus water extract was found higher than the value expected [55.70 +/- 1.59, pyrocatechol equivalent (mu g mg(-1))].
The chemical constituents of the essential oil from aerial parts of Salvia candidissima Vahl., collected in Turkey, were analyzed by GC and GC/MS. The oil yield of the dried plant obtained by hydrodistillation was 0.7 % (v/w). 70 compounds, accounting for 99.65% of the oil, were identified. The major constituents were camphor (28.94%), bornyl acetate (12.80%), borneole (9.44%), beta-cadinene (5.88%), alpha-caryophyllene (5.40%), 1,8-cineole (5.15%), beta-pinene (4.93%) and alpha-pinene (4.89%). In addition, the antioxidant properties of essential oil and hexane, ethyl acetate and ethanol extracts of S. candidissima Vahl. were examined. The antioxidant activity was investigated with two different methods: beta-carotene bleaching test and the 2,2'-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging method. beta-carotene bleaching test shows that the most active extract which were achieved by us were ethanol extract (95,70%) from S. candidissima (94,5%). In DPPH free radical scavenging activities, the ethanol extract (94,55%) and hexane extract (83,21%) were showed high activity, respectively.
The aerial parts of Micromeria juliana (L.) Bentham ex Reichb. were extracted with light petroleum, acetone and methanol, successively. The antioxidant activity of different concentrations of the extracts was evaluated using different antioxidant tests, namely total antioxidant (lipid peroxidation inhibition activity), DPPH (1,1-diphenyl-2-picrylhydrazyl) radical scavenging, ferric reducing power, and metal chelating. Total antioxidant activity was determined using the β-carotene-linoleic acid assay. Unexpectedly, the light petroleum extract exhibited strong lipid peroxidation inhibition activity. The extract was fractionated on a silica gel column and the antioxidant activity of the fractions was determined by the β-carotene-linoleic assay at 25 μg/mL concentration. The fractions that exhibited more than 50% inhibition activity were analysed by GC and GC/MS; thus, the structure of fourteen compounds were elucidated. In addition, acetyl- and butyrylcholinesterase inhibitory activities of the extracts were also determined in vitro. The light petroleum and acetone extracts were found to have mild butyrylcholinesterase inhibitory activity.
The chemical compositions of the essential oils of Salvia potentillifolia (Lamiaceae) were analyzed by GC and GCMS. The oils were obtained by four different methods (hydrodistillation, steam distillation, and two extraction methods) to investigate the effect of temperature on the volatile compounds. In total, 121 components were detected in the various oils. The major compounds characterized were α-pinene (30.2, 31.2, 10.6, and 14.8 %) and β-pinene (15.0, 14.6, 7.6, and 11.4%), respectively. Surprisingly, the percentage concentrations of α-pinene and β-pinene in the hydrodistilled and steam distilled oils were high, even though prepared at high temperature, whereas the contents of both compounds were lower in the essential oils obtained by the extraction methods prepared without added heat. The percentage concentration of 8,13-epoxy-labda-14-en-2-one, a diterpenoid, in the extracted essential oil was 22 times higher than in the hydrodistilled and steam distilled essential oils. However, the concentrations of cis -p-menth-2-en-1-ol was four times, and β-bourbonene and β-caryophyllene two times superior than their percentage concentrations in the hydrodistilled and steam distilled essential oils.