No abstract

No abstract

High performance liquid chromatography in combination with diode array detection (HPLC-DAD) was used to determine morphine, 6-acetylmorphine, cocaine, benzoylecgonine, cocaethylene, methadone and 2-ethylene-1,5-dimethyl-3,3,-diphenylpyrrolidine in human saliva. For comparison, samples were prepared by either liquid-liquid extraction in Toxitubes A or microwave-assisted extraction (MAE), by mixing 1 ml of saliva with 10 ml of chloroform and operating at 100 degrees C for 10 min. Acetonitrile and 0.02 m phosphate buffer at pH 6.5 were used as mobile phase in HPLC in gradient mode. The detector response was linear over the drug concentration range of 0.05-2.0 microg ml(-1) in human saliva. The analytical method was validated by determining its precision and accuracy (n = 5), which were lower than 5% as relative standard deviation and 6% as relative error. Limits of detection ranged from 10 to 35 ng ml(-1); mean recoveries of drugs were from 53 to 95% with Toxitubes A and from 83 to 100% with MAE at two different concentrations (0.1 and 1.0 microg ml(-1)). The proposed method was applied to 24 saliva samples from individuals poisoned with opiates and/or cocaine.

An analytical method is proposed for the simultaneous determination of morphine, codeine, 6-acetyl-morphine (MAM), cocaine, benzoylecgonine (BEG), cocaethylene, methadone and 2-ethylen-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP) in urine using high performance liquid chromatography coupled to a diode array detector (HPLC-DAD). The selection of working wavelengths is based on the highest chromatographic response for each component: 233 nm for cocaine, BEG and cocaethylene; 285 nm for morphine, codeine and MAM; and 292 nm for methadone and EDDP. The mobile phase, which is a mixture of acetonitrile and 0.02 M phosphate buffer at pH 6.53, was eluted in gradient mode through an XTerra RP-8 column (250 mm x 4.6 mm i.d., 5 microm particle size). After applying a solid-phase extraction procedure with Bond Elut Certify cartridges, the recoveries obtained were between 60% (EDDP) and 97% (cocaethylene). A good linearity of the method in the 0.1-10 microg mL(-1) range of urinary concentrations was obtained because the coefficient of correlation exceeded 0.99 for each drug. The precision and accuracy were quite good, with values of <7% and within the range +/- 6%, respectively. Finally, the proposed method was applied to 23 urine samples from fatal intoxications related to methadone, heroin and[sol ]or cocaine.

No abstract