Münevver Açıkkol

Elemental composition of green coffee and its contribution to dietary intake

The concentration of twenty-seven elements (Li, Be, B, Mg, Al, P, K, Ca, Cr, Mn, Co, Ni, Cu, Zn, As, Se, Sr, Mo, Cd, Sn, Sb, Ba, Hg, Pb, Bi, Th, and U) in green coffee samples and their infusions were determined by using inductively coupled plasma-mass spectrometry (ICP-MS). Prior to analysis, green coffee samples were prepared by microwave digestion, while infusions were analyzed without any pre-treatment. The accuracy and precision of the proposed methods were verified by recovery experiments. Considering samples; K, Cu, and Al had the highest mean concentrations with 6714.5μgg(-1), 12.1μgg(-1), and 25.9μgg(-1) among major, trace and toxic elements, respectively. The impact of brewing type on leachability of elements was also studied and the results outlined that mean leachability of elements to Turkish coffee were greater than to mud coffee. Furthermore, dietary element intakes through green coffee consumption were also estimated. This is the first study presenting wide range of elements in green coffee brews and calculating dietary intakes.

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.

Simultaneous analysis method for GHB, ketamine, norketamine, phenobarbital, thiopental, zolpidem, zopiclone and phenytoin in urine, using C18 poroshell column.

Date-rape drugs have the potential to be used in drug-facilitated sexual assault, organ theft and property theft. Since they are colorless, tasteless and odorless, victims can drink without noticing, when added to the beverages. These drugs must be detected in time, before they are cleared up from the biofluids. A simultaneous extraction and determination method in urine for GHB, ketamine, norketamine, phenobarbital, thiopental, zolpidem, zopiclone and phenytoin (an anticonvulsant and antiepileptic drug) with LC-MS/MS was developed for the first time with analytically acceptable recoveries and validated. A 4 steps liquid-liquid extraction was applied, using only 1.000mL urine. A new age commercial C18 poroshell column with high column efficiency was used for LC-MS/MS analysis with a fast isocratic elution as 5.5min. A new MS transition were introduced for barbital. 222.7>179.8 with the effect of acetonitrile. Recoveries (%) were between 80.98-99.27 for all analytes, except for GHB which was 71.46. LOD and LOQ values were found in the ranges of 0.59-49.50 and 9.20-80.80ngmL(-1) for all the analytes (except for GHB:3.44 and 6.00μgmL(-1)). HorRat values calculated (between 0.25-1.21), revealed that the inter-day and interanalist precisions (RSD%≤14.54%) acceptable. The simultaneous extraction and determination of these 8 analytes in urine is challenging because of the difficulty arising from the different chemical properties of some. Since the procedure can extract drugs from a wide range of polarity and pKa, it increases the window of detection. Group representatives from barbiturates, z-drugs, ketamine, phenytoin and polar acidic drugs (GHB) have been successfully analyzed in this study with low detection limits. The method is important from the point of determining the combined or single use of these drugs in crimes and finding out the reasons of deaths related to these drugs.

Madde Kullanımının Kolaylaştırdığı Suçlar: Maddeler ve Etkileri; Deliller ve Analizleri

Deaths by ligature have always been common in the society. The manner of death being suicidal, accidental or homicidal has always been a controversy faced by an autopsy surgeon. Due to the variability of the appearance of the external lesions in different mannerism of mechanical asphyxias the autopsy surgeon is highly dependent upon the history and the circumstances of the death. This study was undertaken in an attempt to identify specific internal lesions in cases of ligature compression of neck. We studied 46 cases of suicidal hanging and 12 cases of ligature strangulation. All the internal lesions were categorized and their correlation was sought in various manner and mode of asphyxia. Strap muscle haemorrhages, laryngeal fractures and tongue bleed were found to be more prevalent in strangulation than hanging. Absence of external injuries points more towards the case being suicidal hanging.

A General Overview of Pesticides in Soil: Requirement of Sensitive and Current Residue Analysis Methods

Pesticides are chemical agents used to destroy or control pests, both in agriculture and in public health. Despite the beneficial effects associated with the usage of them, these chemicals may cause adverse effects to humans and to the nature. In addition, many pesticides are persistent and may therefore bioaccumulate in the environment; also some of them are important carcinogens and mutagens. In the world, alarming levels of pesticides have been detected in air, water, soil, as well as in foods and biological materials. Because of the special character as sink and source of contaminants soil is a critical medium, and as an environmental contaminant that comes into contact with soil intensively, pesticides are one of the important issues of environmental soil forensics. The different classes and wide range of pesticides and environmental mediums containing them have made essential the development of sensitive and current methods for the analysis of pesticide residues for environmental monitoring and forensic investigations. This chapter describes pesticides, historical background of pesticide usage, pesticides classification, environmental impacts and fate of pesticides, misuse and overuse of them, and provides a general brief overview on the soil sampling and pre-treatment, the basic principles of the conventional and also modern extraction approaches (including their advantages and disadvantages), and the chromatographic-based determination techniques used for pesticide residue analysis in soil.

A Highly Specific, Fully Validated Urinary Ethyl Glucuronide Analysis Using Solid Phase Extraction-Liquid Chromatography/Electrospray Ionization-Tandem Mass Spectrometry.

A highly specific and selective analytical method using LC/MS/MS for the quantitative determination of ethyl glucuronide (EtG) in urine was developed and fully validated. Since the determination of EtG in urine may be possible days after the elimination of alcohol, it is an indication of alcohol use in alcohol treatment programs and antemortem and postmortem toxicological investigations. Propyl glucuronide (PrG), which increased the selectivity of the method, was used as an internal standard. The method was validated in terms of selectivity, linearity, LOD, LOQ, intraday and interday precision, and recovery. The analyte and PrG in the SPE cleaned up extract were separated on a 150 mm C18 column in 3.3 min with high resolution. The rest of the peaks from the matrix were eluted in 9.0 min. The LOD was 90.8 ng/mL and the LOQ was calculated using the EURACHEM method as 185.0 ng/mL. The intraday and the intermediate precision of the method was calculated using analysis of variance and confirmed with calculation of HorRat values, which were found within acceptable limits. The method provided a reliable solution for monitoring patients under alcohol addiction treatment and was successfully applied to real samples.