Annex White book.pdf

to the procedure described by Moretti et al. After removing the diluentthrough light nitrogen inflation, the remaining solution is submitted todistillation in vapor stream with alkaline material (NaOH 0,1 N) in a Clevengerapparatus. The oily phase created during the extracting procedureis concentrated in the volumetric part of the apparatus, which containsa certain amount of pure xylol to which a certain amount of phencone(internal standard) has been added. After completion of the essentialoil distillation, the increase of the organic phase is determined. Afterdehydration in anhydrous sodium sulphate the substance is weightedand filled in dark glass containers where it remains at 4 o C until chromatographicdetermination of safranol in a gas phase, which is formedby pricrocrocine hydrolysis, contained in saffron.A4.1.1.6Chromatographic determination of safranol in a gas phaseThe determination is carried out in a Carlo Erba HRSGC Series 5300gas phase chromatograph, equipped with flame ionization detector (FID)connected to a Hewlett-Packard 3396 Series II integrator that containsa connected phase molted silicon capillary column Carbowax 20M (15mm x 0,25 mm, layer thickness 0,25 μm). Analysis is performed in followingconditions: room temperature is programmed by a thermostatto rise from 50 to 180oC, with 3oC /mn rise, initial isotherm 8 mn andinitial phase 20 mn. Injection block and detector temperature is at 200and 220oC respectively. Helium with 0,5 ml/min flow is used as a carrier.The quality determination of safranol is carried out by the use ofthe inner measure. The values obtained in the analyzed samples varybetween 3,83 and 4,82 %.A4.1.1.7Extraction of characteristic components of the substanceThe extraction tests are performed with methanol at a room temperature.In short, 100 mg of dry, oil free substance and exact weightedsubstance are placed in a volumetric distillation bottle that contains25 ml of anhydrous methanol and a magnetic armature. The system isagitated constantly (600 r / min) at a room temperature, unexposed tolight and in nitrogen atmosphere until color residue is formed. Uponcompletion of the extraction procedure, the exhausted substance isseparated from the solution through vacuum filtration and is washed inclear methanol until the washing water becomes colorless. The washingwater is added to the extracted solution until the desired volume of thesolution is reached. The residue is dried in a chamber at 105oC untilweight is stabilized.The values for the dried substance vary around 70% with minimumvalue at 67,73% and maximum value at 72,25%. Bibliography data withreference to the aqueous extract vary from 55% to 60%.144