Development and validation of a cost-effective,efficient, and robust liquid chromatographic method for the simultaneous determination of the acetyl and succinoyl content in hydroxypropyl methylcellulose acetate succinate polymer

A reversed-phase liquid chromatographic method was developed and validated for the determination of the content of free acetic acid, free succinic acid, acetyl substituents, and succinoyl substituents in hydroxypropyl methylcellulose acetate succinate (HPMCAS; Chemical Abstracts Service Registry No. 71138-97-1) polymer. This single new method gave accurate and precise measurement of both acetyl and succinoyl substituents, which had previously required 3 Japanese Pharmaceutical Excipients (JPE) methods to accomplish. Consequently, analysis time and turnaround time are decreased significantly. Furthermore, this method can also separate and determine the free acetic and succinic acids in HPMCAS polymer, a task that the corresponding JPE method cannot achieve. The values for accuracy (average recovery from 12 standard samples) were 99.9% for acetic acid and 99.8% for succinic acid. The values for injection precision (relative standard deviation [RSD]) were 0.11% for acetic acid and 0.28% for succinic acid. The values for intermediate precision (RSD) were 1.25% for determination of the acetyl content at the 8.78% (w/w) level and 1.33% for determination of the succinoyl content at the 10.9% (w/w) level. The values for intermediate precision (RSD) were 5.98% for determination of free acetic acid at the 0.12% (w/w) level and 5.13% for determination of free succinic acid at the 0.029% (w/w) level. The method was proven to be robust with respect to variation in the pH of the mobile phase, the concentration of potassium dihydrogen phosphate, and the flow rate. The method is well suited for quality control in today's fast-paced pharmaceutical laboratories.     

Untersuchungen zur Struktur von 1,1-Komplexen der Nickelhalogenide mit N-substituierten Aminomethyl- und Aminoäthylpyridinen

The 1.1-complexes formed by the reaction of nickel(II) halides and substituted aminoethyl- and aminomethyl-pyridines-(2) may be divided into two groups. Compounds, which are yellow or red brown in the solid state, and violet in solution in acetone belong to the first group. The complexes of the second group are violet in solution and in the solid state. On account of the vis- and ir-spectra, the magnetic behaviour, and the molar weight a distorted tetrahedral structure is discussed for the violet compounds, and a dimeric structure with coordination number 5 of the central atom for the complexes of the first group. The factors determining the structure of the investigated compounds are stated.     

Magnetization reversal of CuyCr2Se4−zBrx single crystals

Due to a partially inhomogeneous Cu concentration, Cu_yCr₂Se_4?zBr_x single crystal can show a complicated temperature dependence of the wall motion threshold field which is about 0.5 kA/m near the Curie temperature. The crystals can be homogenized by means of a NH₄OH treatment.     

Raman and infrared spectra of CdIn2S4 and ZnIn2S4

Four one-phonon Raman lines have been found in CdIn₂S₄ (ZnIn₂S₄) spinels at 92 (72) cm^-1, 186 (184) cm^-1, 246 (253) cm^-1, and 367 (372) cm^-1 for incident photon energies well below the energy gap E_G ～ 2.4 (2.2) eV at 300 K. For photon energies close to E_G, the 367 cm^-1 mode underwent a resonant enhancement in CdIn₂S₄ and four infrared active but Raman forbidden F_1u modes appeared in the CdIn₂S₄ and ZnIn₂S₄ Raman spectra: TO modes at 226 (221) cm^-1 and 309 (312) cm^-1, and LO modes at 274 (272) cm^-1 and 340 (342) cm^-1.     

The Sasaki Hook Is Not a [Static] Implicative Connective but Induces a Backward [in Time] Dynamic One That Assigns Causes

The Sasaki adjunction, which formally encodes the logicality that different authors tried to attach to the Sasaki hook as a ‘quantum implicative connective,’ has a fundamental dynamic nature and encodes the so-called ‘causal duality’ (Coecke et al., 2001) for the particular case of a quantum measurement with a projector as corresponding self-adjoint operator. The action of the Sasaki hook ( $a\xrightarrow{S} - $ ) for fixed antecedent a assigns to some property “the weakest cause before the measurement of actuality of that property after the measurement,” i.e., ( $a\xrightarrow{S}b$ ) is the weakest property that guarantees actuality of b after performing the measurement represented by the projector that has the ‘subspace a’ as eigenstates for eigenvalue 1, say, the measurement that ‘tests’ a. The logicality attributable to quantum systems contains a fundamentally dynamic ingredient: Causal duality actually provides a new dynamic interpretation of orthomodularity. We also reconsider the status of the Sasaki hook within ‘dynamic (operational) quantum logic,’ what leads us to the claim made in the title of this paper. The Sasaki adjunction has a physical significance in terms of causal duality. The labeled dynamic hooks (forwardly and backwardly) that encode quantum measurements, act on properties as $(a_1 \xrightarrow{{\varphi _a }}a_2 ): = (a_1 \to _L (a\xrightarrow{S}a_2 ))$ and $(a_1 \xleftarrow{{\varphi _a }}a_2 ): = ((a\xrightarrow{S}a_2 ) \to _L a_1 )$ , taking values in the ‘disjunctive extension’ $DI(L)$ of the property lattice L, where $a \in L$ is the tested property and $( - \to _L - )$ is the Heyting implication that lives on DI(L). Since these hooks $( - \xrightarrow{{\varphi _a }} - )$ and $( - \xleftarrow{{\varphi _a }} - )$ extend to DI(L)×DI(L) they constitute internal operations. The transition from either classical or constructive/intuitionistic logic to quantum logic entails besides the introduction of an additional unary connective ‘operational resolution’ (Coecke, 2002a) the shift from a binary connective implication to a ternary connective where two of the arguments refer to qualities of the system and the third, the new one, to an obtained outcome (in a measurement)     

Rheological studies of concentrated guar gum

Polymers and surfactants are essential ingredients of the printing paste. Polysaccharides are used commercially to thicken, suspend or stabilise aqueous systems. Also they are used to produce gels and to act as flocculates, binders, lubricants, to serve as modifiers of film properties, and have a function as adjusters of rheological parameters. Surfactants, on the other hand, perform numerous functions acting as dispersants, wetting agents, emulsifiers and antifoaming agents. The rheological properties of polysaccharide thickeners (guar gums with different substitution levels and different producers) at different concentrations and temperatures and, second, the effects produced by the addition of nonionic surfactants (polyoxyethylene stearyl alcohols with different numbers of EO groups) have been studied under linear and nonlinear shear conditions. Experimental data have been correlated with the different models: flow curves with the Cross, Carreau and Meter-Bird model, and mechanical spectra with the generalized Maxwell model and Friedrich-Braun model. The surface tensions of aqueous systems containing polysaccharide and/or surfactants have been determined over extended concentration ranges in order to detect the CMC conditions and to provide a better understanding about the polysaccharide-surfactant interactions.     

Analysis of acrylamide in food by isotope-dilution liquid chromatography coupled with electrospray ionization tandem mass spectrometry

A confirmatory method for the determination of low levels of acrylamide in different food products is presented. The method entails extraction of acrylamide with water, precipitation of matrix constituents with acetonitrile, and two clean-up steps consecutively over Isolute Multimode and cation-exchange cartridges. The final extract is analyzed by liquid chromatography (LC) coupled to positive electrospray ionization tandem mass spectrometry employing [13C3]-acrylamide as internal standard. For the chromatographic step, a LC column based on a polymethacrylate gel is employed which shows good retention of acrylamide under isocratic flow conditions (k' = 1.2). Mass spectral acquisition is done by selected reaction monitoring, choosing the characteristic transitions m/z 72-->55, 72-->54 and 72-->27. In-house validation data for breakfast cereals and crackers show good precision of the method, with intra- and interassay variation below 10%. The limits of detection for crackers and breakfast cereals, respectively are estimated at 15 and 20 microg/kg, and recoveries of fortified samples ranged between 58 and 76%. Furthermore, the method is applicable to a number of different food products, including biscuits, crisp bread, wafers, confectionery cocoa liquor, and nuts. Finally, the good results obtained in several small-scale interlaboratory tests provided additional confidence in the performance of the method.     

Template assisted formation of micro- and nanotubular carbon nitride materials

Micro- and nanotubes of an amorphous carbon nitride material were synthesized by metathesis reactions between cyanuric chloride (C₃N₃Cl₃) and different nitrogen sources, such as Li₂(CN₂) or Li₃(BN₂). The intermediate formation of needle-shaped crystals of N(C₃N₃Cl₂)₃ was always observed in our reactions, and investigated with respect to their role as a template in the formation of tubes. Chemical analyses of the micro- and nanotubes reveal carbon to nitrogen ratios near 3:4, consistent with the suspected material C₃N₄. Synthesized carbon nitride materials were thermally stable up to 600 ^°C in inert atmosphere. They were inspected by a number of physical measurements, mainly using TEM, EDX and IR investigations.