Annex White book.pdf

A4.1.1.2Determination through crude ashesIt is performed pursuant to the description of the European pharmaceuticalindustry, on saffron samples dried at 105 o C in desiccantunit until weight is stabilized. After exact weighing, the saffron sampleis placed in a porcelain capsule and is burned at direct contact to theflame. The weight of the ashes is rendered in percentage of the dry material.All values measured for the San Gavino Monreale production arelower than the highest admissible percentage and vary between 4,98and 5,60 %.A4.1.1.3Determination through n-hexane extractablesIt is performed on saffron thread samples dried at 105oC in desiccantunit until weight stabilized and through a cold treatment with n-hexanein distillery. After extraction, the remaining substance is dried in nitrogenstream and is weighed. The weight difference is rendered in percentagefor 100 g of dried material. Having regards to the traditional techniqueconsisting in soaking the stigmas with extra virgin oil, a cold washing inn-hexane takes place, determining the weight of the extract. The obtainedquantitative data vary between 0,89 and 1,09 %.A4.1.1.4Determination of coloring powerIt is performed pursuant to the description of the European pharmaceuticalindustry, on saffron samples dried at 105oC in desiccantunit until weight is stabilized. These samples are treated afterwards indouble distilled water for a certain period of time. The coloring ability isdetermined through measurement of the transmission optical densityin 440 nm extract solution. The transmission optical density measurementsare performed by a double ray UV-Vis spectrophotometer.A4.1.1.5Safranol extraction and picrocrocine hydrolysis5 g of dried Saffron, fatless and lightly powdered together with 30ml of n-hexane are placed in a 50 ml distiller bottle equipped with mechanicalagitator and deposited coolant. The suspension is agitated at aconstant diluent reflux temperature. It is protected from light exposureand is kept within a small quantity of nitrogen. After three hours, themixture is cooled at a room temperature and is separated through filtrationin 0,45 μm Hewlett-Packard filters cod. HP-5181-1246. The solidanalyte is washed three times with 10 ml diluent. Each time, the washingsolution is mixed with the initial infiltrate. A certain amount of phenconeis added to the succeeded solution that is submitted to chromatographicanalysis in gas form in order to determine the safranol content according143