Determination of strontium in biological samples by atomic emission spectrometry with electrothermal atomization

Summary Strontium showed a high atomic emission in a molybdenum microtube. The addition of hydrogen in the argon gas atmosphere served to increase the atomic emission. No interferences from less than 5 ng of potassium, calcium and magnesium were found. Other elements also had no interferences at the concentration levels usually found in biological samples. Samples were digested with nitric acid in a Uni-Seal decomposition vessel. The results obtained showed good agreement with the certified values. Atomic emission spectrometry with a molybdenum microtube atomizer permits a simple and sensitive determination of strontium in biological samples (coefficient of variation 2.5% for 10 pg Sr).

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Strontiumbestimmung in biologischem Material durch Atomemissions-Spektrometrie mit elektrothermischer Atomisierung

Zusammenfassung Eine hohe Atomemission wurde für Strontium bei Verwendung einer Molybdän-Mikroröhre beobachtet. Durch Wasserstoffzusatz zum Argon konnte sie noch weiter erhöht werden. Weniger als 5 ng K, Ca und Mg verursachen keine Störung. Andere Elemente stören nicht in den Konzentrationsbereichen, wie sie üblicherweise in biologischen Materialien vorkommen. Der Aufschluß der Proben wurde mit Salpetersäure in Uni-Seal-Gefäßen vorgenommen. Die erhaltenen Werte stimmten gut mit zertifizierten Daten überein. Die vorgeschlagene Methode ermöglicht eine einfache und empfindliche Strontiumbestimmung in biologischen Proben (Variationskoeffizient 2,5% bei 10 pg Sr).

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This work was supported by the Ministry of Education, Science and Culture of Japan through a Grant-in-Aid for Special Project Research.     

Novel real-time sensors to quantitatively assess in vivo inositol 1,4,5-trisphosphate production in intact cells

Real-time observation of messenger molecules in individual intact cells is essential for physiological studies of signaling mechanisms. We have developed a novel inositol 1,4,5-trisphosphate (IP(3)) sensor based on the pleckstrin homology (PH) domain from phospholipase C (PLC) delta. The environmentally sensitive fluorophore 6-bromoacetyl-2-dimethyl-aminonaphtalene was conjugated to the genetically introduced cysteine at the mouth of the IP(3) binding pocket for enhanced IP(3) selectivity and for rapid and direct visualization of intracellular IP(3) > or = 0.5 microM as fluorescence emission decreased. The probe, tagged with arginine-rich sequences for efficient translocation into various cell types, revealed a major contribution of Ca2+ influx to PLC-mediated IP(3) production that boosts Ca2+ release from endoplasmic reticulum. Thus, our IP(3) probe was extremely effective to quantitatively assess real-time physiological IP(3) production via those pathways formed only in the intact cellular configuration.     

N-Boc-L-valine-connected amidomonophosphane rhodium(I) catalyst for asymmetric arylation of N-tosylarylimines with arylboroxines

A catalytic asymmetric arylation of sterically tuned imines with arylboroxines was developed by using N-Boc-l-valine-connected amidomonophosphane rhodium(I) catalyst in n-PrOH. The TMS group used for the steric tuning of imines is convertible to other functionalities that are applicable as a key foothold for the carbon-carbon bond-forming coupling reactions.     

Facile synthesis of optically active oxindoles by copper-catalyzed asymmetric monotosylation of prochiral 1,3-diols

A facile synthetic method toward optically active 3,3-disubstituted oxindoles with excellent enantioselectivity was achieved using chiral copper-catalyzed desymmetrization of prochiral 1,3-diols. The monotosylated product was transformed into oxindole derivatives efficiently.     

Ruthenium‐catalyzed fast living radical polymerization of methyl methacrylate: The R?Cl/Ru(Ind)Cl(PPh3)2/n‐Bu2NH initiating system

A fast living radical polymerization of methyl methacrylate (MMA) proceeded with the (MMA)₂? Cl/Ru(Ind)Cl(PPh₃)₂ initiating system in the presence of n‐Bu₂NH as an additive [where (MMA)₂? Cl is dimethyl 2‐chloro‐2,4,4‐trimethyl glutarate]. The polymerization reached 94% conversion in 5 h to give polymers with controlled number‐average molecular weights (M_n's) in direct proportion to the monomer conversion and narrow molecular weight distributions [MWDs; weight‐average molecular weight/number‐average molecular weight (M_w/M_n) ≤ 1.2]. A poly(methyl methacrylate) with a high molecular weight (M_n ～ 10⁵) and narrow MWD (M_w/M_n ≤ 1.2) was obtained with the system within 10 h. A similarly fast but slightly slower living radical polymerization was possible with n‐Bu₃N, whereas n‐BuNH₂ resulted in a very fast (93% conversion in 2.5 h) and uncontrolled polymerization. These added amines increased the catalytic activity through some interaction such as coordination to the ruthenium center. © 2002 John Wiley & Sons, Inc. J Polym Sci Part A: Polym Chem 40: 617–623, 2002; DOI 10.1002/pola.10148     

Synthesis of end‐functionalized poly(methyl methacrylate) by ruthenium‐catalyzed living radical polymerization with functionalized initiators

A series of functionalized 2‐bromoisobutyrates and 2‐chloro‐2‐phenylacetates led to α‐end‐functionalized poly(methyl methacrylate)s in Ru(II)‐catalyzed living radical polymerization; the terminal functions included amine, hydroxyl, and amide. These initiators were effective in the presence of additives such as Al(Oi‐Pr)₃ and n‐Bu₃N. The chlorophenylacetate initiators especially coupled with the amine additive gave polymers with well‐controlled molecular weights (M_w/M_n = 1.2–1.3) and high end functionality (F_n ～ 1.0). © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 1937–1944, 2002     

Six immunosuppressive features from an ascomycete, Zopfiella longicaudata, found in a screening study monitored by immunomodulatory activity

In a screening study on immunomodulatory fungal metabolites, three known anthraquinones, carviolin (roseo-purpurin) (1), 1-O-methylemodin (2), omega-hydroxyemodin (citreorosein) (4), and a new anthraquinone, omega-acetylcarviolin (3), together with a known steroid, ergosta-4,6,8(14),22-tetraen-3-one (5) and a new steroid, 25-hydroxyergosta-4,6,8(14),22-tetraen-3-one (6) were isolated from an Ascomycete, Zopfiella longicaudata, and found to have moderate immunosuppressive activities. The structure-activity relationships of these metabolites are discussed.     

Prenylated xanthones from Garcinia xanthochymus

A new prenylated xanthone, 1,3,5,6-tetrahydroxy-4,7,8-tri(3-methyl-2-butenyl)xanthone (1), was isolated from the wood of Garcinia xanthochymus together with a known xanthone, garciniaxanthone E (2). Their structures were determined by spectroscopic analysis. Compounds 1 (3 microM) and 2 (10 microM) elicited marked enhancement of nerve growth factor-mediated neurite outgrowth in PC12D cells.     

Three lanostane triterpenoids with antitrypanosomal activity from the fruiting body of Hexagonia tenuis

During the search for new antitrypanosomal drug leads, three new antitrypanosomal compounds, hexatenuins A–C (1–3), were isolated from the fruiting body of Hexagonia tenuis. 1 and 3 possessed an unusual malonate half-ester functional group at C-3 position, and 1 and 2 had a spirostructure in the side-chain. Their structures were elucidated using MS analyses, extensive 2D-heteronuclear NMR data interpretation. Compounds 1–3 showed in vitro antitrypanosomal activity against Trypanosoma brucei brucei with IC₅₀ values of 0.57, 8.60 and 5.62 μg/ml, respectively.     

Surface dilational moduli of polymer and blended polymer monolayers spread at air-water interfaces

Surface dilational moduli of polymer monolayers, blended polymer monolayers, and polymer particle monolayers spread at air–water interfaces are reviewed, focusing on measurements using surface pressure isotherm, surface pressure relaxation, and oscillating barrier methods. Differences between the surface dilational moduli of condensed polymer monolayers and expanded polymer monolayers are explored. Moreover, the features of the surface dilational moduli in blended polymer monolayers are discussed in terms of their miscibility.