Guitarrins A-E and Aluminumguitarrin A: 5-Azaindoles from the Northwestern Pacific Marine Sponge Guitarra fimbriata.

Guitarrins A-E (1-5), the first natural 5-azaindoles, and aluminumguitarrin A (1a), the first aluminum-containing compound from marine invertebrates, were isolated from the sponge Guitarra fimbriata. The structures of these compounds were established using detailed analysis of 1D and 2D NMR data, mass spectra, and X-ray analysis of 1 and 1a. Compound 3 was proved to be a natural inhibitor of alkaline phosphatase.

Isolation and Physical Property Optimization of an Amorphous Drug Substance Utilizing a High Surface Area Magnesium Aluminometasilicate (Neusilin(®) US2).

Control and optimization of the physical properties of a drug substance (DS) are critical to the development of robust drug product manufacturing processes and performance. A lack of isolatable, for example, crystalline, DS solid forms can present challenges to achieving this control. In this study, an isolation scheme for an amorphous DS was developed and integrated into the synthetic route producing DS with optimized properties. An inert absorbent excipient (Neusilin® US2) was used to isolate the DS via a novel antisolvent scheme as the final step of the route. Isolation was executed at kilogram scale utilizing conventional equipment. The resulting 50 wt% DS:Neusilin complex had improved physical stability and exceptional micromeritic and tableting properties. Improved dissolution was observed and attributed to enhanced dispersion and increased surface area. Characterization data suggest a high degree of penetration of the DS into the Neusilin, with DS occupying 70% of mesopore and 12% of macropore volume. This approach has application in the isolation and particle engineering of difficult to isolate DS without additional unit operation, such as spray drying, and has the potential for a high degree of optimization and control of physical properties over the course of DS development.

Optimization of alginate purification using polyvinylidene difluoride membrane filtration: Effects on immunogenicity and biocompatibility of three-dimensional alginate scaffolds.

Sodium alginate is an effective biomaterial for tissue engineering applications. Non-purified alginate is contaminated with protein, lipopolysaccharide, DNA, and RNA, which could elicit adverse immunological reactions. We developed a purification protocol to generate biocompatible alginate based on (a) activated charcoal treatment, (b) use of hydrophobic membrane filtration (we used hydrophobic polyvinylidene difluoride membranes to remove organic contaminants), (c) dialysis, and finally (d) ethanol precipitation. Using this approach, we could omit pre-treatment with chloroform and significantly reduce the quantities of reagents used. Purification resulted in reduction of residual protein by 70% down to 0.315 mg/g, DNA by 62% down to 1.28 µg/g, and RNA by 61% down to less than 10 µg/g, respectively. Lipopolysaccharide levels were reduced by >90% to less than 125 EU/g. Purified alginate did not induce splenocyte proliferation in vitro. Three-dimensional scaffolds generated from purified alginate did not elicit a significant foreign body reaction, fibrotic overgrowth, or macrophage infiltration 4 weeks after implantation. This study describes a simplified and economical alginate purification method that results in alginate purity, which meets clinically useful criteria.

Phosphorus recovery as AlPO4 from beneficially reused aluminium sludge arising from water treatment.

The purpose of this study was to develop an efficient and, possibly, a practically operated methodology to recover phosphorus (P) from P-saturated dewatered aluminium sludge cakes (DASC) after the DASC have been beneficially reused as constructed wetlands substrate for P-rich wastewater treatment. A three-step procedure of 1) P extraction by H2SO4, 2) decolorization of extraction leachate via H2O2 oxidation, and 3) AlPO4 precipitation by pH adjustment, has been explored. The optimal conditions to form the precipitates of AlPO4 were determined, with 97% of P and 99% of Al being recovered. The obtained compounds were identified by XRD, FTIR and SEM analyses. Although the purity, structure, characteristics and production control of the compounds are worthy of further investigation, this study provides a showcase of a 'closed loop' regarding the beneficial reuse of a 'waste' and the recovery of useful elements after the reuse.

What do results of common sequential fractionation and single-step extractions tell us about P binding with Fe and Al compounds in non-calcareous sediments?

Correct identification of P forms together with their main Fe and Al binding partners in non-calcareous sediments is of crucial importance for evaluation of P cycling in water bodies. In this paper, we assess extraction methods frequently used for this purpose, i.e., a sequential five-step fractionation (water, bicarbonate buffered dithionite solution (BD), NaOH, HCl, nitric-perchloric acid), ascorbate extraction (pH ~7.5), and oxalate extraction (pH ~3), directly on a range of laboratory prepared Fe and Al minerals enriched with adsorbed P. Extraction selectivity and efficiency for particular P, Fe and Al forms were also verified by specific combinations of these extraction methods applied on freshwater sediment samples. In the sequential fractionation, BD was highly effective in dissolving both amorphous and crystalline Fe (hydr)oxides and the associated P, while neither FeS nor Al (hydr)oxides were dissolved. The following NaOH extraction effectively dissolved both amorphous and crystalline Al (hydr)oxides. The high solubilizing power of BD and NaOH to dissolve crystalline Fe and Al oxides that have only a small P-sorption ability prevents the use of resulting Fe/P and Al/P ratios as simple predictors of total P sorption capacity of sediments and soils. Ascorbate non-selectively extracted small proportions of FeS and amorphous Fe and Al (hydr)oxides, but significant amounts of adsorbed P, which hinders its use for the characterization of P forms in non-calcareous sediments. Similar nonselective characteristics were found for oxalate extractions. As oxalate extracts most of the adsorbed phosphate, it is not possible to use it unambiguously to determine specific Fe/P and Al/P ratios of active complexes. However, this method is convenient (and more selective than NaOH step in the sequential fractionation) for the determination of amorphous Al (hydr)oxides.

Plastic bag method for active sample loading into transmission electron microscope.

A plastic bag method was developed to observe air-sensitive samples on microstructure and phase distribution without exposure to air during the holder transfer process into the transmission electron microscope (TEM). As an example, a type of lithium aluminum hydride (Li(3)AlH(6)) was observed in the TEM to demonstrate the effectiveness of this method. Results show that the plastic bag method is a simple and practical TEM transfer method utilized to reduce air contact for a series of air-sensitive materials.

Identification of particulates in vaccine formulations containing aluminum phosphate.

Density gradient centrifugation was used for identification of particulates in vaccines formulated with aluminum phosphate (AlPO(4)) adjuvant. Protein-derived particulates are sporadically seen in protein pre-filled formulations where siliconized syringes are employed. These particulates are difficult to distinguish from the AlPO(4) suspension. Prior to centrifugation, Histopaque solution is placed at the bottom of the test tube (or the original syringe), resulting in a layer beneath the suspension. After brief centrifugation, AlPO(4) settles to the bottom of the test tube, while the light-weighted particulates in the sample become visible, floating in the inter-phase between the two layers.

Adsorptive micellar flocculation as an efficient method for processing soil extracts containing both surfactant and polychlorinated biphenyls: practical demonstration.

The main purpose of the paper is to share the results and experience from processing soil extracts containing a high concentration of both anionic surfactant and polychlorinated biphenyls (PCBs) by use of method the called adsorptive micellar flocculation. The method is similar to coagulation, but the mechanism is more complicated. The flocculants examined in the laboratory section involved ferric chloride, aluminium chloride, ferric sulfate, and aluminum sulfate. It was observed that ferric chloride provides the best PCB removal efficiency from the extract. Subsequently, two extracts obtained from the pilot-scale demonstration of the PCBs leaching from the soils by the surfactant solution were processed by this method. The volume of the extracts processed was several hundred liters. The method proved it can remove PCBs from all extracts with a very high efficiency (greater than 99.99%). The residual PCB concentrations in solution were less than 1 microg/L.

[Separation and purification of Al13 by chemical precipitation and metathesis].

PACls with different concentrations were prepared by adding sodium carbonate powder into AlCl13 solution. Medium concentration and high Al13 content of PACl was chosen to carry out Al13 separation processes. The influences of SO4/Al molar ratio and the initial total Al concentration on the precipitation reactions of sulfate with different Al species were investigated. The factors influencing the metathesis reaction between solid Al13-SO4 and Ba(NO3)2 were evaluated. Results showed that high Al13 PACl could be obtained at the medium high concentration range of 0.4 - 0.6 mol/L, the optimum SO4/Al ratio was 0.6:1 for precipitation- separation of Al13, Al13 -SO4 precipitates were mostly consisted of tetrahedral crystals. During the metathesis reaction, Ba/SO4 molar ratio of 1:1 is the optimal value. Small range temperature variation and ultrasonic action had no marked influence on metathesis reaction rate and final Al13 concentration. Higher initial Ba(NO3)2 concentration could produce higher concentration Al13 accordingly. The purity of Al13 solution could be reached to 92.1% statistically.