Wastewater-based monitoring of illicit drug consumption in Istanbul: Preliminary results from two districts.

Wastewater-based epidemiology is a well-established and complementary approach for monitoring illicit drug use in the general population. In this study, amphetamine (AMP), methamphetamine (METH), 3,4-methylenedioxymethamphetamine (MDMA), cocaine (COC) (from benzoylecgonine), and cannabis (from THC-COOH) consumption levels were investigated for the first time in Turkey (Istanbul). A solid-phase extraction method was applied to influent wastewater samples collected from two districts, Beyoglu and Catalca. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis was conducted with electrospray ionization in positive mode. Calibration curves were acquired in linear form with >0.999 correlation coefficients. Limit of detection levels were measured as 0.91-151 ng/L, and limit of quantitation levels were in the range of 3 to 500 ng/L. Solid-phase extraction recovery and repeatability experiments were achieved by spiking the mix solution to different concentrations (50, 250, 750 ng/L) in 50 mL tap water and wastewater (500, 1000 ng/L) samples in six replicates. The method was optimized, and recoveries were found to be over 80% for all six substances with up to 11.9% relative standard deviation. According to the real sample results, cannabis was found to be the most abused illicit substance among the analytes. The mean consumptions of the two districts, including seven consecutive days for AMP, METH, MDMA, COC, and cannabis, were found to be 27.2, 322, 331, 385, and 1224 mg/day/1000 inhabitants, respectively. In this presented study, all targeted compounds were analyzed simultaneously with the same analytical conditions. To the best of our knowledge, this report is the first to present illicit drug consumption data from Istanbul.

Report: Fast chromatographic screening method for 7 drugs of potential threat in drug facilitated crimes.

In cases where pharmaceuticals and pharmaceutical candidates are involved in drug facilitated crimes (DFC), like organ theft, robbery, rape and suicides, the analysis of drug powders or solution residues found in crime scenes may give idea on what the victims have ingested. An easy and fast simultaneous determination of 7 drugs; GHB (γ-hydroxybutyrate), GBL (γ-butyrolactone), norketamine, ketamine, fenobarbital, fenitoin and thiopental which have the potential to be used in DFC was performed. The method required no sample preparation and has 12 minutes elution time with a good chromatographic separation. The separation was carried out on a C18 monolithic column with UV detection at 215 and 237nm. All r2 values were ≥0.99 and the linear ranges were between 0.9956-1.0000. The LOD and LOQ values were between 0.56-5.55µgmL-1 and 1.69-16.82µgmL-1 respectively. The repeatability values were <7.35%. This is the first study in the simultaneous screening of the above mentioned drugs using HPLC.

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.

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.

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.