Detection of Cocaine in Seized Drug Samples by Capillary Electrophoresis Tandem Mass Spectrometry
A methodology using capillary electrophoresis with tandem mass spectrometry detection (CE-MS/MS) was developed, and applied to determine the cocaine content of seized drugs. The cocaine separation among other concomitants by capillary electrophoresis was achieved in just 4.0 minutes using 30 mM ammonium formate, pH 6.5, as a background electrolyte (BGE). The correlation coefficient of the calibration curve in the range of 0.02 to 1 μg/mL was upper 0.999, and the limits of detection (LOD) and limits of quantification (LOQ) were 0.003 μg/mL and 0.01 μg/mL, respectively. The relative standard deviation repeatability (intraday and interday) was less than 6.5% (peak area). The analysis of seized suspected illegal drugs revealed the presence of cocaine in 93% of samples (n = 11), in amounts ranging from 0.04 to 429 mg/g, showing a high variability of concentrations of cocaine. The user can change the provider and, due to the large variability of concentration, be lead to an accidental overdose.
Segmental analysis for cocaine and metabolites by HPLC in hair of suspected drug overdose cases.
Hair samples of eight postmortem cases were analyzed in segments of 1 to 3 cm for cocaine, benzoylecgonine and cocaethylene. Samples were prepared for analysis by digestion in 0.1 M HCl and subsequent extraction with mixed-mode solid-phase extraction columns. Measurement was made by reversed-phase, narrow-bore HPLC and fluorescence detection using two laboratory-made internal standards. The concentrations were in the region of 0.29-316 ng/mg of hair for cocaine, 0.43-141 ng/mg of hair for benzoylecgonine and 0.93-1.83 ng/mg of hair for cocaethylene. All eight investigated cases had cocaine-positive segments. In six of the cases, all segments were positive, suggesting regular cocaine use and two showed in-between negative segments indicating an interruption or a change of the abuse intensity. The results showed a second, remarkable observation, i.e. enormous concentration differences (factor >150) for both cocaine and benzoylecgonine between the different subjects. Furthermore, interindividual cocaine/benzoylecgonine ratios ranged from 0.02 to 8.43. We believe these observations could in part be attributed to both some of the still existing limitations in the analytical approach(es), especially the mandatory hair washing steps, and in our still too limited knowledge of the hair incorporation processes. Nevertheless, in some cases, segmental analysis proved to be an important tool to distinguish, together with postmortem examination, deadly chronic abuse from single acute drug overdosage.
Preparation and performance evaluation of swine manure bio-oil modified rubber asphalt binder
Abstract In order to study the effect of the preparation process of swine manure bio-oil modified rubber asphalt binder on the rheological properties of the binder, the matrix asphalt and asphalt rubber were used as the control group, and swine manure bio-oil modified rubber asphalt binders were obtained by three preparation processes. Then the rheological properties of five binders were evaluated by rotational viscosity, DSR, MSCR and BBR tests. The results show that the addition of swine manure bio-oil to asphalt rubber is beneficial to the workability, but cause negative effect on its high temperature performance, fatigue performance and low temperature crack resistance. The preparation method of premixing bio-oil and rubber powder can reduce the degradation of high-temperature performance of asphalt rubber caused by addition of swine manure bio-oil to a certain extent. The fatigue properties of the three bio-binders are close, and the critical temperature is less than 25 °C. The process of premixing bio-oil and rubber powder will increase the creep stiffness and reduce the low-temperature performance. However, the low-temperature performance of the binder obtained by this process is still better than that of the matrix asphalt and can meet the requirements of use. Therefore, it is recommended to use the preparation process of premixing bio-oil and rubber powder to prepare swine manure bio-oil modified asphalt rubber.