High-performance liquid chromatographic determination of morphine and its 3- and 6-glucuronide metabolites: improvements to the method and application to stability studies

Improvements to previously reported methods for the determination of morphine, morphine-3-glucuronide (M3G) and morphine-6-glucuronide (M6G) in human plasma are described. The improved methods involve the use of a solid-phase extraction cartridge and a chromatographic system which uses paired-ion reversed-phase high-performance liquid chromatography with a radially compressed column. Only one cartridge is used to prepare each sample for chromatography and each cartridge may be used for at least fourteen 1-ml plasma samples. The recovery is greater than 85%. The improvements to the method of sample pretreatment and in the chromatographic conditions have allowed determination of morphine, M3G and M6G in human plasma down to 13.3 nmol/l (coefficient of variation = 9.3%), 108 nmol/l (6.6%) and 41 nmol/l (6.7%), respectively, using ultraviolet detection alone. It was shown that all three compounds were stable in plasma for up to 101 weeks when stored at -20 degrees C.     

Self-assembly of a linear mesoscale tetramer with electrical connectivity

Capillary interaction-based self-assembly of block-shaped mesoscale components into an electrically interconnected 1-D tetramer is reported. Low melting point solder droplets, selectively patterned on the faces of the blocks, were employed to drive the sequential alignment, registration, linking and electrical interconnection of each block. The solder patterns were designed so that successful assembly would only occur when the solder patterns on one block face were correctly aligned with those on the face of an adjacent block. For assembly, the blocks were agitated in a flask containing KBr solution. At 60 °C the solder was molten, and collisions between blocks enabled the solder menisci to easily interact. To minimize interfacial free energy, the menisci coalesced and quickly drove the interacting blocks to form a stable, registered and aligned assembly. When agitation was terminated and the solution cooled, the self-aligned, linear tetrameric arrangement of blocks was permanently captured by solder solidification, a process that provided good mechanical bonding and electrical interconnection between each block. PACS 81.16.Dn; 68.03.Cd; 85.40.-e     

The polarographic determination of indium in zinc-base alloys : The determination of indium in zinc and in zinc alloys of low aluminium content

Studies of the application of an 8-hydroxyquinoline extraction and of a zinc oxide “collection” procedure for the separation of trace amounts of indium from zinc alloys are described and discussed. A combination of radio-chemical and polarographic determination were employed for this work. A polarographic method for the determination of indium in zinc and in zinc alloys of low aluminium content is presented     

Effect of varying counterions on the sensitivity of electrohydrodynamic and fast atom bombardment mass spectrometry

The abundance of ion pairs (CA⁺) relative to that of doubly charged ions (C²⁺) in electrohydrodynamic (EH) mass spectra of a series of anions with a common dication in glycerol was found to increase in the order acetate < nitrite < chloride < bromide ≈ nitrate < iodide < perchlorate. Correlation with enthalpies of hydration for the anions suggests that this trend reflects the solution chemistry of ion association. These spectra also reveal that solvation rather than interactions with the extracting field is more important in determining the overall EH mass spectrometric sensitivity to doubly charged ions. Therefore, the use of anions that promote more extensive ion pairing enhances the overall sensitivity to multiply charged ions that otherwise interact strongly with the solvent, but reduces sensitivity to singly charged ions. These observations hold in fast atom bombardment mass spectrometry, surviving the invasive effects of the primary beam.     

1,3,5-Trisubstituted hexahy drotriazines as mannich reagents. I. Preparation of secondary aminomethyl sulfide hydrochlorides

1,3,5-Trisubstituted hexahy drotriazines react with hydrogen chloride in the presence of anhydrous solvents to form useful intermediates for the introduction of the RNHCH₂- group into compounds which undergo the Mannich reaction. The effectiveness of the new aminomethyl-ating agent has been demonstrated by the preparation of secondary aminomethyl sulfide hydro-chlorides.     

Deprotonation-electrophile trapping of terminal epoxides

Organolithium-induced deprotonation of terminal epoxides in the presence of appropriate diamine ligands allows trapping with a range of electrophiles, yielding functionalised di- and tri-substituted epoxides in good yields and with control of stereochemistry at the epoxide.