Liquid chromatography with UV-Vis and mass spectrometric detection (LC-DAD-MS) was applied to the identification of dyes and biological sources in samples from nineteenth to twentieth century ethnographic textiles from ASTRA National Museum Complex, Sibiu, Transylvania. The objects are part of the Romanian traditional costume and are among the first to be acquired for the museum collections, around 1905. Oral and written information mention such objects as homemade, with nearby materials, while literature mentions a significant number of local vegetal sources as being used for textile dyeing. The analytical protocol developed, based on the combined use of the UV-Vis and mass spectrometric detectors to associate the information and distinguish between major and minor dyes, facilitates a clear attribution of the dyes and biological source/sources used. Other techniques, such as X-ray spectroscopy and FTIR-ATR were successfully used to identify inorganic dyes, which may not be detected by LC-DAD-MS, as was the case of Prussian blue. A large number of biological sources was identified in the studied objects, both local and imported. The local sources identified include dyer's broom (Genista tinctoria L.), sawwort (Serratula tinctoria L.), young fustic (Cotinus coggygria Scop.), Rhamnus berries, emodin based dyes (Rhamnus, Rheum, Rumex sp.) and woad (Isatis tinctoria L.), in perfect correlation with literature which states that local dyes were still in use in the period under discussion. Carminic acid containing insects (Dactylopius coccus Costa and Porphyrophora sp.) and redwood type Caesalpinia species should be considered a result of trade. Almost all the natural and synthetic dyes detected are frequently mentioned in a collection of recipes published by the Romanian Academy, in 1914. The richness in colours in belts, the use of insect dyes in shirts decoration and the large amount of cotton in shirts are illustrative for the owners' status. The study provides a better valorisation of the Romanian traditional costume as witness of the rural society at the end of the nineteenth to beginning of the twentieth century and emphasizes the usefulness of chemistry in cultural heritage dedicated applications.
Trimetazidine and internal standard [1-(2,4,5-trimethoxybenzyl)piperazine] were isolated from plasma by protein precipitation with trifluoroacetic acid. The neutralized supernatant was separated on a C(8) column with methanol-aqueous 0.11% triethylamine adjusted to pH 3.3 with formic acid (1:4, v/v) at a flow rate of 0.85 mL/min. The separation was achieved within 8 min and the column ef fluent was transferred into an ion trap analyzer via an atmospheric pressure chemical ionization interface. The mass analyzer was used in the selected reaction monitoring mode, to enhance detection selectivity. The method was fully validated with a quantitation limit for trimetazidine of 1.5 ng/mL. The method was successfully applied to assess bioequivalence of two immediate and two modified commercially available pharmaceutical formulations containing 20 and 35 mg of trimetazidine, respectively.
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