Simultaneous determination of morphine, codeine, 6-acetylmorphine, cocaine and benzoylecgonine in hair by liquid chromatography/electrospray ionization tandem mass spectrometry.

A fast and sensitive liquid chromatography/triple quadrupole tandem mass spectrometry (LC/MS/MS) method was developed for the simultaneous determination of morphine, codeine, 6-acetylmorphine (6-AM), cocaine and benzoylecgonine (BE) in hair. Pulverized hair samples were extracted with methanol, and a 50 microL supernatant aliquot was injected into the LC/MS/MS system. Chromatography was performed with an XBridge phenyl column (3.5 microm particle size, 4.6 x 150 mm), and the mobile phase was composed of methanol and 10 mM ammonium acetate adjusted to pH 4.00 with 99% formic acid (95:5, v/v). A separation run with isocratic elution was completed in 10 min at a flow rate of 500 microL/min. Positive electrospray ionization and multiple reaction monitoring (MRM) with one precursor ion/product ion transition were used for the identification of each analyte. Deuterated analogues as internal standards were used for quantification and qualification. Linearity was established in the concentration range of 100-3000 pg/mg. The limits of detection were 10 pg/mg for morphine, codeine and 6-AM; and 1 pg/mg for cocaine and BE. The precision and accuracy were determined by spiking hair samples at six concentration levels. For all analytes, the relative standard deviations of intra- and inter-day precision were 0.1-6.3% and 1.5-10.6%, respectively. The accuracy ranged from 92.7 to 109.7%. The validated LC/MS/MS method was successfully applied to the analysis of 79 authentic hair samples.

Simultaneous determination of ketamine, tramadol, methadone, and their metabolites in urine by gas chromatography-mass spectrometry.

An automated solid-phase extraction procedure combined with gas chromatography-mass spectrometry methodology, without derivatization, has been developed for the identification and quantitation of ketamine, norketamine, tramadol, methadone, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine, and 2-ethyl-5-methyl-3,3-diphenylpyrroline in urine. The analytical approach is simple and rapid, yet reliable. Good linearity (r(2) > 0.995 over the concentration range of 30 to 600 ng/mL), sensitivity (limits of quantitation 15-30 ng/mL), accuracy (81.0-109.9%), precision (RSD < 13.8%), and recovery (> 79.6% in average) were achieved for all analytes. Ninety-one urine specimens from suspected drug users and 21 clinical urine specimens from methadone substitution therapy patients were analyzed to validate the method compatibility and stability. Results have demonstrated that this GC-MS method is a good confirmation and quantitation test scheme for the six target compounds in urine.

GC-MS quantification of ketamine, norketamine, and dehydronorketamine in urine specimens and comparative study using ELISA as the preliminary test methodology.

An automated solid-phase extraction procedure combined with the gas chromatography-mass spectrometry (GC-MS) methodology, without derivatization, has been developed for the determination of ketamine (K), norketamine (NK), and dehydronorketamine (DHNK) in urine. The analytical approach is simple and rapid, yet reliable, achieving good linearity (r(2)>0.999 over the concentration range of 30 to 1000 ng/mL), sensitivity (limits of quantification = 15, 10, and 20 ng/mL for K, NK, and DHNK, respectively), accuracy (90-104%), and precision (RSD<8.1%) for all analytes. Two hundred and six urine specimens collected from suspected drug users were analyzed by this protocol and also screened by Neogen ELISA method to evaluate the efficiency as well as the compatibility of these two methods. Neogen ELISA showed high efficiency (98.1%), high sensitivity (90.9%), high specificity (98.9%), low false-positive rate (1.1%), and moderate false-negative rate (9.1%), adopting 10 ng/mL K as the cutoff. Neogen ELISA screening followed by GC-MS analysis appeared to be a good screening-confirmation test scheme for the analysis of K in urine. Twenty of the 22 positive urine specimens contained all three analytes simultaneously, with DHNK showing the highest and K the lowest concentrations.

Characteristics and trends of 3,4-methylenedioxymethamphetamine (MDMA) tablets found in Taiwan from 2002 to February 2005.

One hundred and eighty-one 3,4-methylenedioxymethamphetamine (MDMA) containing tablets were sampled from confiscated drugs received by the Taiwan National Bureau of Controlled Drugs for testing from 2002 to February 2005. Sample tablets demonstrated various colors and logos. The appearances, contents of MDMA and other components in these tablets were analyzed in order to understand the characteristics and trends of MDMA use. Samples were analyzed using GC-MS methodology. Deuterated internal standards were used for drug quantification. The MDMA contents varied from 16 to 193 mg/tablet. 66-71% of the tablets seized each year contained only MDMA, and the content of MDMA in MDMA only tablets varied from 89 to 133 mg/tablet. There was a decreasing trend in MDMA content in these tablets over time. Other components commonly found besides MDMA included caffeine (18%), methamphetamine (7%), 3,4-methylenedioxyethylamphetamine (MDEA) (7%) and amphetamine (4%). 3,4-Methylenedioxyamphetamine (MDA), ketamine, ephedrine, diazepam, chlorzoxazone and nicotinamide were also detected. During the study period, the number of other drugs found as well as the combinations of different drugs detected in these tablets increased.