A Validated Chiral LC Method for the Determination of Enantiomeric Purity of Pemetrexed Disodium on an Amylose-Based Chiral Stationary Phase

A simple and new isocratic normal phase chiral HPLC method has been developed for the determination of enantiomeric purity of pemetrexed disodium (l-enantiomer) in bulk drugs with a short run time of about 20 min. Chromatographic separation of l and d-enantiomers of pemetrexed disodium was achieved on an amylose based chiral stationary phase using a mobile phase consists of hexane, ethanol and trifluoro acetic acid. The resolution between the enantiomers was found to be more than 2.0. The system precision and method precision were found to be within 5% RSD for the distomer (d-enantiomer) at its specification level (i.e. not more than 1.0% w/w). The limit of detection and limit of quantification of distomer were 1.6 and 5 μg mL⁻¹, respectively for 10 μL injection volume. The percentage recovery of distomer was ranged from 90.6 to 105.7 in bulk drug samples. The test solution was found to be stable in the diluent for 48 h. The method was found to be specific for the enantiomers of pemetrexed disodium and can be conveniently used for the quantification of undesired d-enantiomer present in the bulk drug samples of pemetrexed disodium.     

Further studies on dynamic crack branching

The newly derived dynamic-crack-branching criterion with its modifications is verified by the dynamicphotoelastic results of dynamic crack branchings in thinpolycarbonate, single-edged crack-tension specimens. Successful crack branching was observed in four specimens and unsuccessful branching in another. Crack branching consistently occurred when the necessary conditions ofK _I =K _{I b} =3.3 MPa \(\sqrt m\) and the sufficiency condition ofr _o =r _c =0.75 mm were satisfied simultaneously. In the unsuccessful branching test, the necessary condition was not satisfied sinceK _I was always less thanK _{I b} .     

The impact of the natural sciences on archaeology

This article reviews some of the applications of physics to the solution of archaeological problems. The use of magnetic, resistivity and electromagnetic surveying techniques for the location of buried features is described. Various methods of age determination are outlined while the problems associated with radiocarbon dating of organic material and thermoluminescent dating of pottery are discussed in detail. The techniques, including petrological examination, chemical analysis and isotopic analysis, employed in the physical examination of archaeological artefacts are described. Examples of the application of these techniques in establishing the source of the raw materials used in pottery, metal and stone implements and in elucidating the techniques of manufacture of pottery and metal objects are also given.     

Small surface and corner crack propagation in aluminum and steel alloys

The purpose of the investigation reported here was to examine experimentally the transition behavior of a short crack in detail using surface-crack measurements with a traveling microscope and micromeasurements obtained by scanning-electron microscopy (SEM). The cyclic growth and transition of initial part-through cracks into through the thickness flaws are documented through experiments by using compact-type specimens fabricated from 7075-T6 aluminum, 2024-T3 aluminum, and mild-steel material, with a keyhole notch. Paper was presented at the 1986 SEM Fall Conference on Experimental Mechanics held in Keystone, CO on November 2–5.     

Analysis of the waterjet contact/impact on target material

Numerical modeling via finite element analyses (FEA) and experimental measurements via moiré interferometry were applied to the investigation of abrasive waterjet (AWJ) drilling. Polycarbonate and alumina blocks with dimensions of 25.4 mm×19.5 mm×6.25 mm were subjected to concentrated static loads experimentally and numerically. The assumptions of the FEA model are verified by comparing the experimental results with the numerical solution. A closed-form solution confirmed the correlation between the two. It was concluded that the assumption of the FEA model (e.g. mesh, boundary conditions, pressure loading, etc.) represented the static conditions. This conclusion allowed the application of a hybrid numerical/experimental technique to understand the complex interaction of the target material and the AWJ slurry column during drilling.     

Phenolic compounds,essential oil composition,and antioxidant activity of Angelica purpurascens (Avé-Lall.) Gill

In this study, methanol extracts (MEs) and essential oil (EO) of Angelica purpurascens (Avé-Lall.) Gill obtained from different parts (root, stem, leaf, and seed) were evaluated in terms of antioxidant activity, total phenolics, compositions of phenolic compound, and essential oil with the methods of 2,2-azino-bis(3ethylbenzo-thiazoline-6-sulfonic acid (ABTS•⁺), 2,2-diphenyl-1-picrylhydrazil (DPPH•) radical scavenging activities, and ferric reducing/antioxidant power (FRAP), the Folin–Ciocalteu, liquid chromatography−tandem mass spectrometry (LC−MS/MS), and gas chromatography-mass spectrometry (GC−MS), respectively. The root extract of A. purpurascens exhibited the highest ABTS•⁺, DPPH•, and FRAP activities (IC₅₀: 0.05 ± 0.0001 mg/mL, IC₅₀: 0.06 ± 0.002 mg/mL, 821.04 ± 15.96 µM TEAC (Trolox equivalent antioxidant capacity), respectively). Moreover, EO of A. purpurascens root displayed DPPH• scavenging activity (IC₅₀: 2.95 ± 0.084 mg/mL). The root extract had the highest total phenolic content (438.75 ± 16.39 GAE (gallic acid equivalent), µg/mL)). Twenty compounds were identified by LC−MS/MS. The most abundant phenolics were ferulic acid (244.39 ± 15.64 μg/g extract), benzoic acid (138.18 ± 8.84 μg/g extract), oleuropein (78.04 ± 4.99 μg/g extract), and rutin (31.21 ± 2.00 μg/g extract) in seed, stem, root, and leaf extracts, respectively. According to the GC−MS analysis, the major components were determined as α-bisabolol (22.93%), cubebol (14.39%), α-pinene (11.63%), and α-limonene (9.41%) among 29 compounds. Consequently, the MEs and EO of A. purpurascens can be used as a natural antioxidant source.     

Edge Finishing Effects on the Impact Behavior of Chopped GFRP Composites

The low velocity and low energy impact response of two common sheet mold compound (SMC) material systems—SMC-R27, and SMC-R37—were investigated. In addition to characterizing the low velocity impact response and failure progression of the material systems, the edge effects of diamond saw cutting, waterjet cutting and abrasive waterjet cutting were investigated using optical microscopy and contact surface profilometry. Impact force–time and displacement–time responses were measured and used to characterize energy absorption capabilities and potential correlation to post processing operation and fiber volume fraction. Pre and post-impact edge surface micrographs were examined to relate the failure behavior on the machined surfaces. Experiments and measurements all show that the failure zone size and growth behavior are clearly dependent on the edge finishing process.     

Investigation of displacement fields in an abrasive waterjet drilling process: Part 1. Experimental measurements

The transient state of displacement fields in the machining zone of a target material during abrasive waterjet impinging and drilling was investigated. A moiré interferometry experimental setup for recording displacement fields and a dynamometer for measuring the reaction force were developed. Whole fields of surface displacement fields and the reaction force of the ceramic and polycarbonate target materials were successfully recorded when the specimen was being pierced by high-pressure abrasive waterjet (AWJ). This paper demonstrates that bothu andv displacement fields of a workpiece during AWJ drilling can be recorded in real time and simultaneously by the moiré interferometry experimentation. The measured surface displacement distributions and the machining forces will be used to drive a finite element model in the second part of this investigation, in which the authors study the stress and strain state for the target material associated with the jet-materials interaction during the jet penetration process.     

Transition Metal Ion-binding Properties of a 14-Membered N2O2S2- Macrobicyclic Ligand

The selective liquid–liquid extraction of various transition metal cations from the aqueous phase to the organic phase was carried out using a 14-membered N₂O₂S₂-macrobicycle. Metal picrates such as Pb²⁺, Co²⁺, Zn²⁺, Ni²⁺,Cu²⁺ and Cd²⁺ were used in this extraction studies. It was found that the ligand showed moderate selectivity towards Pb²⁺ only among the other metals. The extraction constant (log K _ex) was determined to be 13.8 for Pb²⁺ complex.