Zeynep Türkmen

Cytotoxic Activity of Some Anatolian Salvia Extracts and Isolated Abietane Diterpenoids

Abstract Salvia hypargeia. Fisch. et Mey. (Lamiaceae) root extract, among 16 Salvia. extracts, showed the highest activity against the human ovarian cancer cell line. Bioactivity-guided fractionation of this plant extract has yielded four abietane-type diterpenes [5,6-didehydro-7-hydroxytaxodone (1), 14-deoxycoleon U (= 6-hydroxysalvinolone) (2), demethylcryptojaponol (3), and salvicanaric acid (4)] two triterpenes (lupeol and lupeol-3-acetate), and a fatty acid mixture consisting mainly of palmitic acid (51.6%) and palmitoleic acid (6.4%). Compounds 2 and 3 were found to be active against A2780 human ovarian cancer cell line with IC50 values of 3.9 and 1.2 μ g/mL, respectively, and the fatty acid composition was the most active part of the extract (IC50 = 0.6 μ g/mL).

Quantitative lead determination in coating paint on children׳s outwear by LA-ICP-MS: A practical calibration strategy for solid samples

Lead is a hazardous compound that affects the central nervous system in people, particularly children, and may cause some reversible and irreversible diseases. Legal regulations try to prevent the exposure from products especially produced for children such as coating paints, jewelry, toys, bed linen, textile, etc. The aim of this study was to determine the lead levels of coating paints on children׳s outwear selling in district bazaar by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and to specify the percent of non-complying samples. Here we described the solid matrix calibration method and confirmed the results with the microwave-assisted acid digestion method. Both comparative methods were validated by analysis of the certified reference materials (NIST SRM-612 glass matrix, NIST SRM-2582 powdered paint and ERM-EC681k) and bias% for accuracy and RSD% for precision were calculated lower than 6.8% and 7.3%, respectively. The recovery ranges of laser ablation and microwave-assisted acid digestion method for Pb were found to be between 88.2-98.1% and 95.3-101.3%, respectively. The limits of detection values were determined as 0.162 mg kg(-1) for direct sampling in the ablation chamber and 0.002 ng mL(-1) for aqueous solutions. Correlation result of 16 samples (r=0.99) examined in both methods was satisfactory. In coating paint samples, 14.65% of 198 (n=29) did not comply with the 90 mg kg(-1) lead limit according to regulation. Validated quantitative laser ablation method may be preferred to quickly and reliably determine the Pb levels in other solid samples as well as coating paints.

A new clerodane diterpene and other constituents from Ajuga chamaepitys ssp. laevigata

Abstract From Ajuga chamepitys ssp. laevigata, a new clerodane diterpene, ajugalaevigatic acid, has been isolated besides five known compounds, a diterpene, (13S)-15-hydroxylabd-8(17)-en-19-oic acid, a steroidal glucoside, 3-O-β -D-glucopyranosyl-stigmasta-5,25-diene, and triterpenes,α- and β -amyrin and ursolic acid. Their structural elucidation is based on NMR and MS spectroscopic analyses. For the new compound 2D NMR experiments were carried out. Ajugalaevigatic acid was tested against a panel of cytotoxic cell lines, and only found to be active against the A2780 human ovarian cancer cell line.

Determination of α-cypermethrin from soil by using HPTLC

α-Cypermethrin is a synthetic pyrethroid insecticide used to control insects. In soil, α-cypermethrin biodegrades relatively slowly under both aerobic and anaerobic conditions. A high-performance thinlayer chromatography (HPTLC) method was developed for the determination of α-cypermethrin from soil by microwave-assisted extraction (MAE). The linearity range was between 12.5 and 1000 ng/spot, the limit of detection was 2.1 ng/spot, the limit of quantification was 6.4 ng/spot, and the recovery was 91%. The reported method was found to be sensitive, rapid, and suitable for the analysis of α-cypermethrin in soil and it was successfully applied to the soil samples collected from a treated agricultural field. α-Cypermethrin was detected in all soil samples at concentrations ranging from 78.9 to 708.7 ng g−1.

An HPTLC Method for the Determination of Oleandrin in Nerium Plant Extracts and Its Application to Forensic Toxicology

The study reported in this paper was aimed to develop an accurate, specific, and precise high-performance thin-layer chromatography (HPTLC) method for the determination of oleandrin in Nerium oleander (Linn.) extracts as well as biological samples of an intoxication case for the first time. Also, extraction, isolation, and purification methods of oleandrin from the sticky juice of Nerium plant leaves were presented. The retention factor (RF value) of oleandrin was found to be 0.24 ± 0.01. The linearity range was between 2 and 75 ng spot−1 (r = 0.9993), the limit of detection was 2.2 ng spot−1, the limit of quantification was 6.7 ng spot−1, and the recovery in urine and serum was found 89% and 83%, respectively. Isolated compounds from both plant material and biological samples were also applied to mass spectrometry (MS). The reported HPTLC method was sensitive, rapid, and suitable for the analysis of oleandrin and was applied to a non-fatal case of oleander poisoning. Oleandrin was detected in urine and serum samples of the intoxicated patient at concentrations of 3.2 and 8.4 ng mL−1, respectively. Peak purity of the isolated compound was checked by electrospray ionization-mass spectrometry (EI-MS) and introduced to HPTLC compound library. To the best of our knowledge, this study is the first published HPTLC method and also presents the evaluation of both clinical and toxicological aspect of an oleander posioning case. It can be successfully applied for the determination of oleandrin in clinical and forensic researches as well as in phytochemical investigations.

Development and validation of a densitometric-high-performance thin-layer chromatographic method for quantitative analysis of amitriptyline in gastric lavage

Drug overdose is the most common method in suicide attempts. Amitriptyline (AMT), a tricyclic antidepressant agent, known for potentially lethal cardiovascular and neurological effects, is used especially by intoxicated patients. The aim of this study was to validate a method for the determination of AMT in gastric lavage samples by high-performance thin-layer chromatography (HPTLC). Artificial gastric lavage was used to obtain a better extraction procedure for AMT. The method was also applied to patients who attempted suicide with AMT. A validated, accurate, and rapid HPTLC-based method was developed for quantitation of AMT in gastric content of intoxicated patients. Extraction was done from 3 mL gastric lavage sample by liquid-liquid extraction procedure with ethyl acetate-n-heptane (1:1, w / w) in alkaline pH with 10.8. The mobile phase was an isocratic solvent system consisting of methanol-ammonia (25%) (98.5:1.5, v / v). 3,4-Methylenedioxy-Nmethamphetamine (MDMA) was used as internal standard (IS). Analytes were quantified by TLC Scanner operating under 209 nm. The retardation factors of AMT and MDMA were determined as 0.49 and 0.25, respectively. The analytical range was set as 10–250 ng spot−1 for AMT. Calibration was linear within the selected range in gastric lavage (r > 0.9995). Limit of detection and limit of quantification of AMT were found to be 5.1 and 17.3 ng spot−1, respectively. Recoveries of 25 ng spot−1 and 100 ng spot−1 concentrations were found 83.12% and 91.89%; bias% values were 10.91 and 3.19, respectively. The validated method was also applied on samples of five patients who attempted suicide by AMT, and concentrations in gastric lavage samples of 5 patients were found 7.1, 8.3, 9.9, 14.6, and 36.6 ng mL−1. This successfully validated method was applied to suicide cases, and it can be conveniently employed on both antemortem and postmortem cases suspected by amitriptyline.

Current Problems in the Use of Illegal Substances Ingredients

It is known that many diluents and adulterants are used to make illegal substances appear in larger amount and bring more profit. Identification of such additives in illegal substances is particularly important, since some of the toxic effects of such compounds are much more harmful than impact of illegal substances used. The unpredictable substances may endanger the lives of illegal substance users. In this study, the content of two samples brought with suspected illegal substance were investigated and in Sample 1, paracetamol, caffeine and griseofulvin, other the hand in Sample 2 phenacetin were determined as adulterants. Increasing of the contents and ratio of the adulterants in these illegal substances day by day, it should be considered that these additives should also be taken into account in the case of an unexpected death or permanent damage. The findings were evaluated with the groups who have done similar studies in terms of change in content of adulterants and possible health risks, which they may caused.