OBJECTIVE: To develop a column-switching high-performance liquid chromatographic method for the determination of morphine and O6-monoacetylmorphine in urine. METHODS: Urine samples (1.0 ml) were spiked with 1.0 ml borate buffer, after centrifugation, 1.0 ml of supernate were injected directly into an extraction column (YWG C18 33 mm x 5.0 mm, 10 microns). After a washing step with the extraction mobile phase, the retained morphine and O6-monoacetylmorphine were flushed into the analytical column (Lichrospher 100 CN 125 mm x 4.0 mm, 5 microns) with the mobile phase CH3OH-H2O (60:40). The analytical mobile phase is CH3OH-phosphate buffer (pH6.86) (22:78). The UV detector was set at lambda 286 nm. RESULTS: The method shows excellent linearity from 50 to 1,600 ng/ml for morphine and from 100 to 1,600 ng/ml for O6-monoacetylmorphine. The linear correlation coefficients were > 0.999. The relative standard deviations were < 4%. The limits of detection were 40 ng/ml for both morphine and O6-monoacetylmorphine. CONCLUSION The method described is sensitive, rapid, reproducible, and simple.
Chromatography, High Pressure Liquid/methods* ; Heroin Dependence/urine* ; Humans ; Morphine/urine* ; Morphine Derivatives/urine* ; Sensitivity and Specificity

OBJECTIVE: To propose a method for simultaneous determination of codeine(COD), 6-monoacetyl-morphine (6-MAM), morphine (MOR), morphine-3-glucuronide (M3G) and morphine-6-glucuronide (M6G) in human urine by ultra performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS). METHODS: After precipitation of protein by acetonitrile, the urine samples, with added the morphine-d3 (MOR-d3) and morphine-3-Glucuronide-d3 (M3G-d3) as internal standards, were pre-treated by Sirocco protein precipitation plate, and then analyzed by UPLC-MS/MS. RESULTS: The limit of detection was 0.2 ng/mL for both COD and MAM, the limit of quantitation was 0.5 ng/mL for both COD and MAM. The limit of detection was 0.5 ng/mL for MOR, M3G and M6G, the limit of quantitation was 1 ng/mL for them. The linear correlation coefficients were not less than 0.9997, both the inter-day and intra-day precisions were less than 10%, the recoveries were in the range of 70.0% to 98.3%, the matrix effects were about 50.5% to 99.0%. CONCLUSION This proposed method is simple, rapid and accurate, it could be applied in forensic toxicological analysis.
Chromatography, Liquid/methods* ; Codeine/urine* ; Humans ; Limit of Detection ; Morphine/urine* ; Morphine Derivatives/urine* ; Reproducibility of Results ; Sensitivity and Specificity ; Substance Abuse Detection/methods* ; Tandem Mass Spectrometry/methods*

OBJECTIVE: To compare morphine and codeine concentration in urines of heroin abusers and codeine users and to discuss the judgment index to distinguish between heroin abuser and codeine user. METHODS: The urines of heroin abusers and codeine users were collected at different time periods. After protein precipitation, the urine samples were conducted for the qualitative and quantitative analysis of morphine and codeine by UPLC-MS/MS. And the results were all statistically analyzed. RESULTS: Statistical analysis showed that morphine and codeine concentration in urines of heroin abusers and codeine users were both abnormal distributions. The probability of the heroin abuser would be more than 95% and less than 5% for the codeine user when the concentration of morphine in urine sample was more than 67 ng/mL. The probability of the codeine user would be more than 95% and less than 5% for the heroin abuser when the concentration of morphine in urine sample was less than 67 ng/mL. CONCLUSION The morphine concentration in urine could be used as a criterion to distinguish the heroin abuser from the codeine user, while the codeine concentration could not.
Administration, Oral ; Chromatography, High Pressure Liquid ; Codeine/urine* ; Forensic Toxicology/methods* ; Heroin Dependence/urine* ; Humans ; Morphine/urine* ; Solutions ; Substance Abuse Detection/methods* ; Tandem Mass Spectrometry/methods*