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In this manuscript we aimed at the simultaneous separation and quantification of Gemcitabine and Irinotecan hydrochloride (injected both as single components and in combination) from Sprague Dawley rat plasma by using a validated method obtained through the use of a High Performance Liquid Chromatography (HPLC)-diode array detector (DAD). Gemcitabine and Irinotecan hydrochloride were detected and quantified using a Zorbax Extend C-18 column (250 mm × 4.6 mm; 5 μm particle size) in gradient elution mode. The chromatographic analyses were carried out in 15 min. The analytical mode was calibrated and validated in the concentration range from 0.1 to 18 μg/mL both for Gemcitabine and Irinotecan hydrochloride. Sprague Dawley rat plasma was used to perform the analysis. 3-methylxanthine was the internal standard. The weighted-matrix matched standard curves of Gemcitabine and Irinotecan hydrochloride showed a good linearity up to 18 μg/mL. Parallelism tests were also performed to evaluate whether the over-range samples could be analyzed after dilution without affecting the analytical performance. The intra- and inter-day precision (RSD%) values of Gemcitabine and Irinotecan hydrochloride were ≤7.14% and ≤11.5%, respectively. The intra- and inter-day trueness (Bias%) values were in the range from -11.5% to 1.70% for both drugs. The analytical mode performance was further tested after collecting Sprague Dawley rat plasma following a single-dose administration of chemotherapeutics or their association. The validated HPLC-DAD method allowed the simultaneous quantification of Gemcitabine and Irinotecan hydrochloride in the rat plasma, besides the evaluation of the pharmacokinetic parameters and drug delivery.

The di-isonitrilopalladium(O) compounds: Pd(RNC)2 (R = phenyl, p-tolyl, p-anisyl) in which the metal is in a formal zero oxidation state, have been prepared. These compounds are of a type different from the ones with Ni and Cr as metals, e.g. Ni(RNC)4 and Cr(RNC)6, previously described by the author, and probably have a polymeric structure.

This is a cross-sectional study with a randomized choice of individuals aiming at studying the validity of the Brazilian biological exposure limits applied to lead level in the blood (PbB) and delta-aminolevulinic acid in the urine (ALAU), which are 60 mu/dl and 10 mg/g.creat., respectively. Thus, twenty workers, whose PbB and ALAU values have been below these limits over the past two years, were selected at random at a battery plant in the State of S. Paulo, Brazil. The workers were submitted to a variation of the WHO Neurobehavioral Core Test Battery. The results were compared with those obtained for workers of a control group also chosen at random. The lead workers showed memory, mood and motor coordination disorders. Comparing these results with those obtained from the control group, a significant difference was observed (p-value0.02). The results indicate that the Brazilian biological exposure limits above should be reconsidered.

The reaction of Ir4(CO)12 with potassium hydroxide in methanol and/or with sodium in tetrahydrofuran leads to the carbonyliridate anions [HIr4(CO)11]−, [Ir6(CO)22]2−, [Ir8(CO)20]2−, [Ir6(CO)15]2− and [Ir(CO)4]− obtained as salts with bulky cations. From these, the tetranuclear carbonyl hydride H2Ir4(CO)11 and the hexanuclear carbonyl compound Ir6(CO)16 are also obtained.

The reaction of IrH3(PPh3)3 with p-anisyldiazonium tetrafluoroborate gives an insertion product which very easily undergoes orthometalation, yielding [IrH(PPh3)3NHNC6H3OMe]+BF4− (V), the structure of which is tentatively assigned. By reaction with halides X−, the metalated fluoborate gives the neutral IrHX(PPh3)2NHNC6H3OMe, which with halogens X2 affords IrX2(PPh3)2NHNC6H3OMe, the structure of which has previously been determined.

The preparation of Ir2(CO)6(PPh3)2 by a new route is described, as are the reaction of this compound with hydrogen, mercury, tin(II) chloride, hydrogen halides and halogens, leading to new monophosphine carbonyl iridium compounds. The [Ir(CO)3PPh3]- anion has been isolated as the tris(phenanthroline)nickel salt.

The compounds obtained by reaction of 2-alkenols with tricarbonylbis(triphenylphosphine)iridium cation in basic medium, are alkenyloxycarbonyl derivatives, in which the alkenyloxycarbonyl moiety is chelated through a σ and a η bond.

In this paper the author reviews the work carried out under his direction in the laboratory of the Italian Research Council on the structure of an unusual class of compounds in which metal atoms in zero or low oxidation states are bonded to one another. The resolution of the configuration of the atoms in these interesting compounds may well improve our understanding of the electronic structure of metals and alloys.

New platinum derivatives, having oxidation number zero, with triarylphosphines, triarylarsines, triarylphosphites are described. Some of these compounds are coordinatively saturated, i. e. of the type Pt°(PAr3)4, other are unsaturated, of the type Pt°(PAr3)3. The phosphine derivatives reacts with carbon monoxide giving mixed carbonyl-phosphine derivatives.

New cluster gold compounds with 1,2-bis((diphenylphosphino) ethane (DPe) are described. These belong to the following types: (1) The ionic brown compounds Y = Cl−, Br , I−, SCN−, CIO4−, PF6− and BPh4−. (2) The polymeric red violet no-ionic green copounds [Au6(DPE)3]X2. Conductivity measurements, infrared spectra and exchange reactions seem to indicate in these compounds the presence of gold custers of six atoms.

The reaction of K2IrBr6 with carbon monoxide at high pressure yielded the previously unknown K2[Ir2(CO)4Br5]. From this, by condensation, cleavage and oxidation reactions, a number of halocarbonyl anions were obtained, which were isolated as tetraphenylarsonium and tetrabutyl-ammonium salts, namely: [Ir(CO)2Br2]−, [Ir2(CO)4Br3]−, [Ir2(CO)4Br4]−, [Ir(CO)2Br3]− From the reaction of K2IrCl6 with carbon monoxide at high pressure the nonstoicheiometric salt K2[Ir2(CO)4Cl5−e] was obtained, and from this, K[Ir2(CO)4Cl4] and H[Ir2(CO)4Cl4] were prepared. The mode of formation and the possible structure of these halogenocarbonyliridates are discussed.

Tetra-isonitrilo-kobalt(II)-komplexe der Zusammensetzung [CoY4]X2 (Y = aromatisches Isonitril, X = J, ClO4), gehen in Losung beim Erwarmen (z. T. schon bei Raumtemperatur) oder unter der Einwirkung von Reduktionsmitteln in die bestandigen Komplexe [CoY5]X uber. Diese Verbindungen des einwertigen Kobalts sind Durchdringungskomplexe mit abgeschlossener Elektronenkonfiguration. Alle untersuchten Verbindungen sind diamagnetisch.

Die Arylisonitrilo-nitrosylverbindungen Fe(NO)2(CNR)2 und Co(NO)(CNR)3 wurden auf verschiedenen Wegen dargestellt. Sie sind recht stabil und konnen durch Umfallen aus organischen Losungsmitteln leicht rein dargestellt werden. Selbst wenn man annimmt, das das Stickoxyd als [NO]+ koordiniert wird, ergibt sich auf Grund des Elektronegativitatsunterschiedes zwischen Metall und Stickstoff eine Ladungsverteilung der MeN-Bindung, die der der MeC-Bindung in den Metallcarbonylen sehr ahnlich ist.

By reaction of NaBH 4 on [LAuCl] (L = PPh 2 Et in ethanol solution [L 2 Au 3 Cl. H 2 O] 4 was obtained and [L 4 Au 6 Cl] Y (Y = ClO 4 , PF 6 , BPh 4 . On the basis of the IR spectra, molecular weights and conductivities structure are proposed for the above compounds having clusters with three gold atoms.

After a brief summary of the role played by immunity in preventing the development of malignant neoplasms, the AA. in a speedy sequence treat of tumoral markers and their possibilities in diagnostic use. Then AA. make a precis of trials of different types of immunotherapy and as well of researches object of future therapeutic use.

A unique case of chorionic carcinoma of the right frontal lobe of the brain with extensive subarachnoid and intracerebral hemorrhage is presented. No pelvic or pulmonary findings by physical or X-ray examination were present. The craniotomy, irradiation and chemotherapy effected a cure. A nephrectomy was necessary during the postoperative period.

The iridium complexe hydrides so far reported, belong to the type IrH3L3, where L may be triphenylphosphine (1) or the diethylphenylphosphine (2). Using as ligand triphenylphosphine we have now prepared the unsaturated hydride IrH3L2, as well as the hydridocarbonylphosphineiridium compounds IrHCOL2, IrH3COL2, IrH(CO)2L2 and IrHCOL3.

New class of carbonyliridium derivatives is, described, that is the halogenocarbonyliridiates of the types: K[Ir(CO)2Cl2,5]; K[Ir(CO)Br3]; K[Ir(CO)Br4].

The compound [{Ir(CO)3(PPh3)}2](1) reacts with P(OPh)3 to give [{Ir(CO)2[P(OPh)3]2}2] from which [{Ir(CO)3[P(OPh)3]}2] may be obtained. Compound (1) also gives [Ir2(CO)5(PPh3)3] with PPh3, [Ir2(CO)5{PPh2(C6H4Me-p)}2(PPh3)] with PPh2(C6H4Me-p), and [{Ir(CO)2(PPh3)(SO2)}2], having two bridging sulphur dioxide molecules, with SO2. Reaction of the last compound with hydrogen gives [{Ir(CO)2H(PPh3)}2SO2] and reaction with iodine gives [{Ir(CO)2(PPh3)I2}2SO2], having two bridging and two terminal iodine atoms and one bridging sulphur dioxide molecule, but no metal–metal bond. The compounds [{Ir(CO)2[P(OPh)3]2}2] and [{Ir(CO)3[P(OPh)3]}2] and sulphur dioxide gives [{Ir(CO)[P(OPh)3]2(SO2)}2] and [{Ir(CO)2[P(OPh)3](SO2)}2] respectively in each of which a metal–metal bond is postulated.

(Alkoxycarbonyl)iridium compounds of type [Irl2(CO2R)(CO)L2] have been prepared by the reaction of K[Ir(CO)2l4] with nitrogen bases L and alcohols ROH. The reaction takes place through nucleophilic attack of the alcohols on the intermediate cations [lrl2(CO)2L2]+, some of which have been isolated. Other (alkoxycarbonyl)iridium compounds containing triphenylphosphine (Y), [Irl2(CO2R)(CO)Y2] and [Irl(CO2R)(CO)2Y]2 were obtained by the reaction of [Irl(CO)2(Y2)] and [lr(CO)3Y]2 respectively with iodine and alcohols.