Alkylation of ethylenethiourea with alcohols: a convenient synthesis of S-alkyl-isothioureas without toxic alkylating agents

The alkylation of ethylenethiourea with alcohols and aqueous acids (HCl, HBr, and HI) allows the synthesis of the respective S-alkyl-isothioureas in high yield and purity. Consistently high yields (91-98%) were obtained with 56% HI, the yields for 48% HBr (48-93%) and 37% HCl (36-85%) were lower and varied with the type of alcohol. The method is a convenient low-cost alternative to the use of alkyl iodides and an easy access to the S-tert-butyl isothiourea.     

Analysis of bufadienolides in the Chinese drug ChanSu by high-performance liquid chromatography with atmospheric pressure chemical ionization tandem mass spectrometry

The qualitative analysis of bufadienolides in the Chinese drug ChanSu was performed using high-performance liquid chromatography with atmospheric pressure chemical ionization tandem mass spectrometry (APCI-MS/MS). Bufadienolides are the major bioactive constituents of ChanSu, which is used to treat heart failure and cancer in traditional Chinese medicine. The APCI-MS fragmentation behavior of bufadienolides was studied. For bufadienolides with only hydroxyl substituents, the fragmentation was characterized by successive eliminations of H(2)O and CO molecules, and the profile of MS/MS product ions was correlated with the number of hydroxyl groups. If a C-16 acetoxyl group was present, the fragmentation of [M+H](+) ions was triggered by initial loss of 60 Da (HOAc). The elimination of CO was significant for bufadienolides with a 19-formyl group, and the 19-hydroxyl group could be characterized by the loss of 30 Da (HCHO). These fragmentation rules were applied to the identification of bufadienolides in a methanolic extract of ChanSu, which was separated on a C(18) column with gradient elution. A total of 35 bufadienolides were identified, including four new constituents. The method established here facilitated the convenient and rapid quality control of ChanSu crude drug and its pharmaceutical preparations.     

The in vivo neutron activation analysis of calcium in the skeleton of normal subjects,with hypokinesia and bone diseases

A facility developed for the in-vivo neutron activation analysis (IVNAA) of calcium in some parts of tubular limb bones, in the hand, foot and spine is described. The⁴⁸Ca(n, )⁴⁹Ca reaction is used, the gamma-rays of⁴⁹Ca (E=3.08 MeV, T_1/2=8.8 min) are measured. The irradiation is carried out with five of ten²³⁸Pu–Be neutron sources with a source stength of 5·10⁷ n s^–1 each arranged in a bath filled with water. NaI(T1) detectors (from 2 to 4 in number) of 150×100 mm size supplied with lead and shadow shielding are used in the counting unit. The construction of the facility started in 1972 and has been in operation since 1974. It has been used for the examination of patients suffering from limb bone tumors, of children with rickets-like and similar diseases and for studies in space medicine.     

Application of a novel micro-injector in the determination of indole derivatives in the rat pineal gland by capillary electrophoresis with electrochemical detection

A novel micro-injector has been fabricated for capillary electrophoresis (CE). It was successfully used for the determination of some indole derivatives for example melatonin (MT), serotonin (5-HT), tryptophan (Trp), and 5-hydroxy-tryptophane (5-HTrp) in the rat pineal gland by capillary electrophoresis with electrochemical detection (CE-EC). CE was performed in 0.20 mol L(-1) phosphate buffer (pH 8.0). The compounds investigated can be well separated and detected within 15 min. The working electrode used was a 300-microm diameter carbon electrode positioned opposite the outlet of the capillary. The relationship between peak current and analyte concentration was highly linear in the range from 0.10 to 500 micromol L(-1); detection limits (S/N = 3) were 0.03-0.13 micromol L(-1). The proposed method has been successfully used to analyze real biological samples.     

Surface ablation by excimer laser irradiation of Ti and Ti6Al4V alloy

This paper presents the surface microstructure of Ti and Ti6Al4V alloy irradiated with a high output energy XeCl ( = 308 nm) excimer laser. The treatments are carried out on both materials at two beam fluences and the effects of single- and multiple-pulse irradiation are compared. The results of the scanning electron microscopy and of the X-ray diffraction techniques suggest the possible influence of both time-behaviour and energy fluence of the laser pulse on the relative weight of the ablation rate and of the reaction product deposition rate at the sample surface.