Evaluation of the degree of mixing of combinations of dry syrup, powder, and fine granule products in consideration of particle size distribution using near infrared spectrometry

We used near infrared (NIR) spectroscopy to evaluate the degree of mixing of blended dry syrup (DS) products whose particle sizes are not specified in the Revised 16th Edition of the Japanese Pharmacopoeia, and also evaluated the degree of mixing when powder products or fine granule products were added to DS products. The data obtained were used to investigate the relationship between the particle size distributions of the products studied and the degree of mixing. We found that the particle size distribution characteristics of the 15 DS products studied can be broadly classified into 5 types. Combinations of frequently prescribed products were selected to represent 4 of the 5 particle size distribution types and were blended with a mortar and pestle. The coefficient of variation (CV) decreased as the percent mass of Asverin? Dry Syrup 2% (Asverin-DS) increased in blends of Periactin? Powder 1% (Periactin) and Asverin-DS, indicating an improved degree of mixing (uniformity). In contrast, in blends of Periactin and Mucodyne? DS 33.3%, mixing a combination at a 1:1 mass ratio 40 times resulted in a CV of 20%. Other mixing frequencies and mass ratios resulted in a CV by 50% to 70%, indicating a very poor degree of mixing (poor uniformity). These results suggest that when combining different DSs, or a DS with a powder or fine granule product, the blending obtained with a mortar and pestle improves as the particle size distributions of the components approach each other and as the ranges of the distributions narrow.     

Magnetic Susceptibility of Deintercalated Tunnel Compound of KxCr5Se8 and Mössbauer Spectra of Kx(Cr0.95 57Fe0.05)5Se8

Abstract

KCr₅Se₈ has a TIV₅S₈-type structure, containing K ions in one-dimensional tunnels. Deintercalated samples of K_xCr₅Se₈ (0.32 ≤ x ≤ 0.93) were prepared by leaching method using Alc₃/FeCl₃ aqueous solution. These samples showed a broad peak of magnetic susceptibility at ca. 130 K. ⁵⁷Fe-Mössbauer spectra of K_x(Cr_0.95 ⁵⁷Fe_0.05)₅Se₈ (x = 1.0, 0.49) showed a quadrupole doublet at 300 K. Magnetic sextets appeared at 4.2 K in both samples, indicative of magnetic ordering. The observed isomer shift indicated that the charge of Fe is +3 in both samples. It was proposed that Se^2- was partially oxidized by the deintercalation.     

A switchable molecular rotator: neutron spectroscopy study on a polymeric spin-crossover compound

A quasielastic neutron scattering and solid-state (2)H NMR spectroscopy study of the polymeric spin-crossover compound {Fe(pyrazine)[Pt(CN)(4)]} shows that the switching of the rotation of a molecular fragment--the pyrazine ligand--occurs in association with the change of spin state. The rotation switching was examined on a wide time scale (10(-13)-10(-3) s) by both techniques, which clearly demonstrated the combination between molecular rotation and spin-crossover transition under external stimuli (temperature and chemical). The pyrazine rings are seen to perform a 4-fold jump motion about the coordinating nitrogen axis in the high-spin state. In the low-spin state, however, the motion is suppressed, while when the system incorporates benzene guest molecules, the movements of the system are even more restricted.     

Reaction efficiency of organic alkalis with various classes of lipids during thermally assisted hydrolysis and methylation

Reaction efficiencies of two organic alkalis, tetramethylammonium hydroxide (TMAH) and trimethylsulfonium hydroxide (TMSH), with lipids during thermally assisted hydrolysis and methylation (THM) were examined focusing on (1) the types of lipids and (2) degree of unsaturation of fatty acid moieties. Different types of lipids such as triglycerides, phospholipids, free fatty acids and cholesteryl esters containing saturated, monounsaturated or polyunsaturated fatty acid (PUFA) residues were subjected to THM-gas chromatography (GC) in the presence of TMAH or TMSH. The obtained results revealed that the THM reaction using TMAH allowed almost quantitative methylation of saturated and monounsaturated fatty acid components independently of the classes of lipids. However, strong alkalinity of TMAH brought about isomerization and/or degradation of PUFA components. In contrast, the use of TMSH was effective to highly sensitive detection of PUFA as well as saturated and monounsaturated fatty acid components contained in triglycerides, phospholipids (phosphatidylcholines) and free fatty acids. On the other hand, TMSH was proved to react hardly with any kind of fatty acid residues in cholesteryl esters due to their steric hindrance.     

Metallic Contaminant Detection using a High-Temperature Superconducting Quantum Interference Devices Gradiometer

We develop magnetic metallic contaminant detectors using high-temperature superconducting quantum interference devices （HTS-SQUIDs） for industrial products. Finding ultra-small metallic contaminants is an important issue for manufacturers producing commercial products such as lithium ion batteries. If such contaminants cause damages, the manufacturer of the product suffers a big financial loss due to having to recall the faulty products. Previously, we described a system for finding such ultra-smafi particles in food. In this study, we describe further developments of the system, for the reduction of the effect of the remnant field of the products, and we test the parallel magnetization of the products to generate the remnant field only at both ends of the products. In addition, we use an SQUID gradiometer in place of the magnetometer to reduce the edge effect by measuring the magnetic field gradient. We test the performances of the system and find that tiny iron particles as small as 50 × 50 μm^2 on the electrode of a lithium ion battery could be clearly detected. This detection level is difficult to achieve when using other methods.     

A Twist‐Assisted Biphenyl Photosensitizer Passable Through Glucose Channel

While the development of low‐molecular‐weight drugs is saturating, agents for photodynamic therapies (PDTs) may become alternative seeds in pharmaceutical industry. Among them, orally administrative, cancer‐selective, and side effect‐free photosensitizers (PSs) that can be activated by tissue‐penetrative near‐infrared (NIR) lights are strongly demanded. We discovered such a PS from scratch by focusing on a twist‐assisted spin‐orbit charge transfer intersystem crossing (ISC) mechanism in a biphenyl derivative, which was demonstrated by thorough photophysical studies. The unique ISC mechanism enables the PS to be small and slim so as to pass through glucose transporters and exert a PDT effect selectively on a cancer cell line. The smallness will allow for oral administration and fast clearance, which have been agenda of approved PSs with larger molecular weights. We also demonstrated that our PS was able to be activated with an NIR pulse laser through two‐photon excitation.     

Isotope shift measurements of 11, 9, 7Be+

We have performed precision atomic spectroscopy of trapped radioactive Be isotopes aiming at studies of the charge and magnetization radii of these nuclei especially for a single-neutron halo nucleus ¹¹Be . Some experimental results and the status of the analysis are discussed.     

On-column isomerization of sugars during high-performance liquid chromatography: analysis of the elution profile

Four monosaccharides (glucose, galactose, mannose and fructose) and one disaccharide (maltose) were subjected to high-performance liquid chromatography with UV or refractive index detection. Various profiles such as broad, tailed and splitted peaks were produced, depending on column temperature and eluent flow-rate because these saccharides underwent isomerization. In contrast, -methylglucoside, a non-converting derivative, always produced a sharp peak. By analyzing these profiles kinetic constants of the isomerization were obtained and compared with the literature data.