Urgent first-step screening method for ketamine, phenobarbital, zopiclone, zolpidem, phenytoin and thiopental in adulterated soft drink.

Date-rape drugs given to victims through drinks without their knowledge in drug-facilitated sexual assaults and thefts (money, property and body organs), are important threats for the public. Detection in beverage residues gains importance, since some of them can be quickly eliminated from the body, till the victim understands what he/she has experienced, goes to the hospital and gives a urine sample for analysis. Here, date-rape drugs; ketamine, thiopental, phenobarbital, zolpidem, phenytoin and zopiclone were analyzed simultaneously in 1.00mL caffeine-based carbonated beverage residue, through direct injection, using a modified, economical emergency first-step screening method with high performance liquid chromatography-diode array detector (elution time: 11 minutes). Screening power of the method was qualitatively observed in sour cherry juice, sweet soda and beer with some additional experiments. Caffeine in caffeine-based carbonated beverage could also be detected simultaneously. LODs and LOQs were between 0.02-1.79 and 0.08-5.60µgmL-1. Repeatability and reproducibility values were <9.91%. HorRat values were between 0.184-0.500. As the first screening and quantitative study on the simultaneous analysis of these drugs in a beverage, it's important for solving the crimes committed using drugs in caffeine-based carbonated beverage residues found at the crime scene, when the use of these drugs is suspected after anamnesis and inspection.

Speedy Gonzales analysis method in one drop of beverage, for crimes committed with drugs from three different groups.

Sertraline, zolpidem and fentanyl, are drugs with potential to be used in cases of rape, property theft and organ theft. In this study, a 15 min dilute-and-shoot analysis method was developed for the simultaneous confirmation and quantification of these drugs, using liquid chromatography tandem mass spectrometry (LC-MS/MS), in the residues of fruit juice types (mixed fruit juice, cherry juice and apricot juice), frequently consumed soft drinks. A C18 phenomenex column (3 µm × 100 mm × 3 mm) was used in LC-MS/MS analysis. Validation parameters were determined by means of linearity, linear range, LOD, LOQ, repeatability and intermediate precision studies. The linearity of the method was shown up to 2.0 µgmL-1 concentration and r2 was ≥ 0.99, for each analyte. LOD and LOQ values were found in the ranges of 4.9-10.2 and 13.0-57.5 ngmL-1 for all the analytes. Accuracies were between 74 and 126%. HorRat values calculated (between 0.57 and 0.97), revealed that the inter-day precisions (RSD% ≤ 15.5%) are acceptable. The simultaneous extraction and determination of these analytes in beverage residues in very low amounts as 100 µL is challenging because of the difficulty arising from the different chemical properties, the complexity of mixed fruit juice matrix. The method is important for hospitals (especially in emergency-toxicology cases), criminal and special laboratories from the point of determining the combined or single use of these drugs in drug facilitated crimes (DFC) and finding out the reasons of deaths related to these drugs.

Who touched the document?: A new overall strategy for collection and identification of DNA from the questioned documents as a supportive evidence.

The questions on which judges/prosecutors apply for expertise are mostly about by whom a document was drafted/signed. In this study, a new collective strategy was constructed including a collection method, a modified-silica-based DNA isolation method, and a novel purification method on four contact traces formed on four different paper surface during writing, using PCR with AmpFlSTR®GlobalFiler™ STR kit (after experimental comparison between three different kits) and identification using CE. This collective analysis approach is more sensitive and superior to its equivalents on questioned documents in literature because quantifiable amounts of touch DNA and profiles with high loci percentages (100% on day 1, 72.72% after 1 week) were obtained up to 1 week even after the most challenging conditions of sample forming that a forensic scientist can meet; as washing hands just before drafting and using a very low pressure in a shorter time (simulating a simple contact real conditions while drafting), using no visualizing technique that damages the document. Using the strategy, four most commonly used paper types were compared, to see in which of them DNA could be recovered better. The success of this strategy was shown on the 1-day to 10-year-old real samples from a diary and some archive documents from a law office (including the mix-DNA and different ballpoint pens). Thus, it became possible to show if a person had touched the document, in high success rates up to 1 week as a secondary evidence, when primary evidences are insufficient for the detection of document fraud offenses.

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.

A Fast Liquid Chromatography Tandem Mass Spectrometric Analysis of PETN (Pentaerythritol Tetranitrate), RDX (3,5-Trinitro-1,3,5-triazacyclohexane) and HMX (Octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine) in Soil, Utilizing a Simple Ultrasonic-Assisted Extraction with Minimum Solvent.

Direct analyses of explosives in soil using liquid chromatography tandem mass spectrometry (LC-MS/MS) methods are very limited in the literature and require complex procedures or relatively high amount of solvent. A simple and rapid method was developed for the determination of pentaerythritol tetranitrate (PETN), 3,5-trinitro-1,3,5-triazacyclohexane (RDX) and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX), which are among the explosives used in terrorist attacks. A one-step extraction method for 1.00 g soil with 2.00 mL acetonitrile, and a 8-min LC-MS/MS method was developed. The detection limits for PETN, RDX and HMX were 5.2, 8.5 and 3.4 ng/g and quantitation limits were 10.0, 24.5, 6.0 ng/g. The intermediate precisions and Horwitz Ratio's were between 4.10 - 13.26% and 0.24 - 0.98, in order. This method was applied to a model post-blast debris collected from an artificial explosion and real samples collected after a terrorist attack in Istanbul. The method is easy and fast and requires less solvent use than other methods.

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.

Spectrophotometric investigation of the chemical compatibility of the anticancer drugs irinotecan-HCl and epirubicin-HCl in the same infusion solution.

The use of infusional chemotherapy, especially in an ambulatory setting, absolutely requires that the individual agents remain stable in solution at room temperature and that the drugs be compatible. Because of this, investigation of the chemical compatibilities of chemotherapeutic drug combinations given in the same infusion solution is quite important especially if the drugs are to remain in solution for long periods. Thus, the visual and chemical compatibility of irinotecan and epirubicin in the same infusion solution were investigated using both reference standards and pharmaceutical dosage forms. No sign of incompatibility was observed upon visual examination by means of effervescence, pH change, precipitation and colour change. But a chemical incompatibility was observed using a spectrophotometric method in the spectra of irinotecan-HCl and epirubicin-HCl. The molar ratio of epirubicin-HCl/irinotecan-HCl at which the interaction reached a maximum was found to be 2:1. The chemical interaction occurred immediately after admixing and no visual or spectral change was noticed for 24 h after the interaction had occurred. It is concluded that these drugs are chemically incompatible. While the applicability of these two drugs in combination is investigated in further pharmacological studies, their chemical interaction should also be a consideration. The positive or negative contribution of this interaction to the pharmacological effect of the combination might be of importance, and therefore should be investigated in further clinical trials.