Proton magnetic resonance spectroscopic determination of disulfiram: collaborative study

A proton magnetic resonance spectroscopic method for determining disulfiram in the bulk drug product and in the formulated material was collaboratively studied. The method depends on the use of chloroform-d as a solvent and hexamethylcyclotrisiloxane as the internal standard. No interference from tablet excipients was observed. The method is rapid and specific. Eighteen laboratories analyzed duplicate samples of a bulk drug product, a 250 mg tablet composite, and a 500 mg tablet composite. The average per cent results and standard deviations were 99.7 +/- 1.4, 100.9 +/- 2.0, and 99.9 +/- 2.2, respectively.     

Analysis of fat-soluble vitamins. XXIII. High performance liquid chromatographic assay for vitamin D in vitamin D3 and multivitamin preparations.

Vitamin D is determined in preparations containing other fat-soluble vitamins by high performance liquid chromatography (HPLC). The unsaponifiable residue is extracted and separated from interferences by reverse phase chromatography; the fraction corresponding to vitamin D3 is collected and quantitated using normal phase chromatography (amylalcohol-n-hexane as mobile phase) by measuring the vitamin D3 and pre-vitamin D3 peaks at 254 nm. Previtamin D3 content is calculated as vitamin D3 with a conversion factor (determined on the equipment used). Application of the method to vitamin AD3 mixtures in oils gives 98-102% recovery. The reproducibility, using an external standard, is 2-3%, calculated as the coefficient of variation; with an internal standard, the coefficient of variation is 1-1.5%. The method measures potential vitamin D3 content in preparations containing greater than or equal to 200 IU/g in the presence of all known vitamin D3 isomers, vitamin A, and vitamin E.     

The effect of propionic acid on the storage losses of hay

Storage losses in moist hay treated with propionic acid were compared with those occurring in untreated moist hay in two experiments and with field-cured hay in three experiments. Dry matter losses in treated hays ranged from 41 to 8.6% and from 1.7 to 12.6% in untreated hays. Digestible organic matter losses in both treated and untreated hays were generally greater than dry matter losses. Only in one experiment did propionic acid application significantly reduce nutrient losses in moist hays. Nutrient losses, and water-soluble carbohydrate losses in particular, were shown to be correlated with maximum and cumulative bale temperatures during storage in two of the experiments. The rise in hale temperatures during storage was reduced in all three experiments, to a greater or lesser extent, by application of the additive. Loss of propionic acid from the hay during and after application was very large. In the three experiments 86.2, 85.3 and 85.6% of the acid applied was lost by the end of the storage period. Acid distribution studies indicated that variation in acid concentration within bales was as great as between bales. It was concluded that more research is needed into applicator design and position on the baler and into alternative application methods if the benefits of propionic acid as a moist hay preservative are to be fully exploited.     

Mineralogisch-chemische umwandlungen bei der verwitterung pyroklastischer gesteine auf teneriffa (Kanarische Inseln)

In a weathering profile on pyroclastic material four phases of volcanic activity could be defined by mineralogical analysis. Halloysite in 10 Å- and 7 Å-modifications is the predominant new mineral formed by weathering processes. Various degrees of development of this clay-mineral were found in scanning microscopy.The paragenesis of gibbsite, ilmenite and anatase is characteristic for horizons of most intense weathering. The gibbsite found in distinct layers indicates an alteration of climatic conditions between eruption-stages 3 and 4. Absolute age determinations on potash-felspars from a layer of stage 3 yield 1.53 mio. years (+ 10%).     

An Experiment to Control Fomes annosus in Second Rotation Pine Crops

Stump removal was found to singnificantly reduce killing byFomes annosus in second rotation crops of pine. Poisoning andgirdling of trees prior to felling and also stump poisoningfailed to control the disease. In this experiment no significantdifferences were detected in the susceptibility of Scots andCorsican pine to attack. Increasing periods of delay beforereplanting resulted in less mortality. An equation is presented,based on factors of the first rotation crop which may be usedto predict losses likely to occur when a site is replanted.Root attack by F. annosus results in reduced growth and yieldas well as mortality. The results from the experiment are discussed in trems of themangement of pine crops attacted by F. annosus in Theford Chase.