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Measuring mass percentage of degree of moisture in saffron:
 M0: Initial weight of saffron and plate M1: Secondary weight of saffron and plate Note: Maximum mass percentage of moisture and volatile materials is 12 for saffron. Measuring saffron total ash based on dry materials:
M0: Weight of vacant crucible (initial weigh of crucible) M2: Weigh of crucible and ash (crucible final weight) M: Saffron sample amount based on gr. = 1 A: Ash percentage H: saffron moisture percentage Note: Maximum mass percentage of total ash is 7 according to dry substance. Measuring insoluble ash percentage in HCL based on dry substance: 1- Pour 25 cc choleridric acid (HCL) (1 + 3) on ash obtained from determined stage of total ash percentage, 2- One clock glass should be placed on crucible and let it be boiled for a period of 20 minutes. 3- Let crucible be cooled for a while (at temperature of environment) 4- Through the application of Watt man filter paper No. 42, it is strained in 250 cc burette (or ash-free strainer paper). Filter paper should be washed with distilled water, aimed at excluding it from acidity property. Note: For authenticity and accuracy of complete wash, silver nitrate in small amount is poured in a burette. Filter drops are poured in it. If it did not turn color of milk, we continue up to the next stage, otherwise, filter paper should be washed enough, aimed at not change color of silver nitrate. 5- Then, filter paper is burned at the same previous crucible. 6- The crucible containing burned paper should be placed inside furnace at 550 degree of centigrade as long as its color is turned white. 7- Then, it is placed in desiccators for a period of 30 minutes. 8- Crucible should finally be weighed. 9- Percentage of insoluble ash in HCL is calculated according to dry substance at the sample as follows:
M0: weight of vacant crucible (initial weight of crucible) M1: weight of crucible and ash (crucible final weigh)
A100: Percentage of insoluble ash in HCL H: percentage of moisture of saffron B: percentage of insoluble ash in HCL based on dry substance, Note: Maximum mass percentage of insoluble ash in acid is 1.5 based on dry substance. Note 1: Strainer paper, used in iron, should be reached up by fixed weigh and weighed at cooled desiccators. Note 2: Acid should be added to water for the provision of acid. Measurement of mass percentage of solvent substances at cold water (essence) based on dry substance 1- Weighing one gr. of rubbed saffron from the taken sample, 2- Pouring saffron in burette 100, 3- Pouring 50 cc distilled water inside burette, 4- Blending liquid inside burette for a period of 2 hours, once every 20 minutes, 5- Voluming liquid inside burette after 2 hours and holding it fixed for a period of 18 hours in a dark place, 6- Straining liquid in 250 cc burette with strainer paper (540) Wattman 7- Taking out 25 cc of strained liquid with bubbled pipette and pouring it in a plate which has been reached a fixed weigh. Its weight has been noted down previously. 8- Placing plate on water bath with the aim of drying it, 9- Placing plate inside oven in 105 degrees of centigrade for a period of one hour, 10- Placing plate in desiccators with the aim of cooling it, 11- Weighing plate 12- Mass percentage of solution substances in cold water (essence) based on dry substance at the sample is calculated as follows:
M0: weight of initial plate M1: weight of plate and essence A: Amount of solution in cold water in gr. H: percent of moisture of saffron B: mass percentage of solution substance in cold water according to dry substance Note: mass percentage of essence is 65 at large according to dry substance. Determination of existence of additive color according to polyamides method: 1- Weighing and rubbing 5% gr. saffron from made sample and passing from sieve with mesh (500 micrometer), 2- Transferring prepared sample to centrifuged pipe and pouring Ml10 distilled water (c60) on it, 3- Blending and mixing sample with glassy blender for a period of 10 to 12 minutes, 4- Placing in centrifuge device for a period of 13 minutes (3000 circle per minute) 5- Preparing SPE column: placing one filter inside column, adding 14% and 16% gr. polyamides powder and placing second filter on it. Then, place syringe on column and add 10ml distilled water to it (with pump in wire) 6- Separation of sample phase inside centrifuge to separate dish and adding 25.0 cc formic acid to it, 7- Transferring saffron solution to purification column (pump free) 8- Washing stages start after completion of sample inside column. All washing stages with turn on or off pump is made as follows: 9- 30cc distilled water, 30cc methanol, 30cc acetone and 30cc methanol (pump free or with pump in wire) 10- Related pipe is placed at below part of pertinent column and column, containing sample, is washed with ammonia methanol (95 percent). (pump free) 11- Tube containing sample should be evaporated in boiling water. 12- Adding 5.0 cc methanol to the container containing evaporated sample 13- Injecting ul10 of container containing sample on TLC 5577 paper and/or on TLC 5553 paper, 14- Placing TLC paper inside tank containing solvent. 15- Solvent on TLC paper is heightened. In case of existence of coloring, their additional is separated: solvent formulas: Solvent No. 1: tri-citrate sodium 2 gr. + 80 ml distilled water + 30 percent ammonia in weight (ml 20) Solvent No. 2: HCL (Chloridric potassium) 4.0 gr. + 38 ml distilled water + tri-butane 50 ml + pro-biotic acid m1 12 Note: Artificial color should not exist at any rate in saffron. Determining No. of Saffron Pigments 1- Making alcohol 80% (80 cc alcohol 96 degrees, 16 cc distilled water) 2- Weighing and rubbing 1.0% gr. saffron from made sample, 3- Adding 4 cc alcohol 80 to 1% saffron and covering it with foil up to 24 hours, 4- Injecting 1% micron or one micro liter of this solution on TLC 5553 paper and placing it in special solvent, 5- Heightening solvent up to 10 cm in an chromatography tank, 6- Counting the number of appeared spots, measuring at 6, and measuring their distance up to injection line and dividing it to 10. Formula of Solvent: 4 volume of buthanol + 1 volume of acetic acid + 1 volume of distilled water (40 cc) + 10 cc + 10 cc Note: The number of pigments of saffron should be measured at 6 at large. 7-upon heightening solvent in height of screen, various materials are also enhanced but with different speed. Determining Crosin, Picro-Crosin and Safranal in Saffron 1- Rubbing the amount of approx. one gr. of saffron from made sample and sieving it with mesh (500), 2- Weighing 5% gr. of sieved saffron, 3- Pouring this amount of saffron on a 100 cc burette with approx. 850 cc distilled water, 4- Placing burette inside aluminum foil for preventing it from being exposed to light, 5- Placing burette on magnetic blender for a period of one hour with 1000 circle per minute, 6- Volumizing liquid obtained in a 1000 cc phial (Wrapped in aluminum foil) 7- Taking out 20 cc of the liquid and pouring it in a 200 cc Erlenmeyer and volumizing it with distilled water 8- Straining liquid obtained by vacuum pump of air reservoir and silicate straining paper (cellulose acetate with diameter of 45% micrometer) 9- Preparing spectrophotometer (turn it on half an hour in previous) 10- Reading numbers and figures of the device in length of waves (330, 257 and 440 nanometer) which indicate amount of crosin, picro-crosin and safranal. 11- Amount of crosin, picro-crosin and safranal of saffron is calculated as follows: divide read figures for each part into 0.005 and multiplication is made for dry substance. h: percentage of moisture of saffron and the least bitterness of picro-crosin at wave length of 257 nanometer includes:
The rate of aroma, fragrance and flavor of safranal at the wave length is 330, including: the least 20 and maximum 50 and the least power of coloring (crosin) at the wave length (440 nanometer) includes:
Maximum of mass percentage of azotes based on dry substance: 1- Weigh one gr. of sample saffron in a strainer paper and twist strainer paper on its round, and then, content is poured into kejdal balloon. 2- Then, 10 gr. of potassium sulfate and one gr. copper sulfate is added to the catalyst and then 25-cc thick sulfuric acid is added to them. 3- Then, the device is mounted and thick NaoH is poured inside part of it up to half part. 4- The, the third part is put on it and flare should be turned on. Note 1: Flare should be heightened gradually and little by little. Note 2: All these operations should be made under extractor fan. It should be noted that some glassy pearl was also added in the beginning to kejdal balloon. 5- After fizzing and soothing, solution of flare is enhanced gradually. 6- When solution turned into green color, let it be heated up to half an hour, with the aim of exclusion of all gases and its steams. Then, it should be taken out from temperature. 7- Then, distillation stage is started and the device should be installed. 8- We need laboratory balloon containing solution at this stage. 9- 50 cc, 1.0, normal HCL and 25 cc distilled water and some drop (agent of bermocerosel green) is spilled inside recipient Erlenmeyer Flask (at the right hand of device) Note: Reagent 0.083 gr. bermocerosel green and 0.016 gr. methyl should be poured inside joje balloon (100) and then, it must be reached to a volume with alcohol. 10- Erlenmeyer Flask should be placed over the jack at the right hand of the device in such a way that tube of the device should be placed completely inside acid. Jack should be lowered a little every often. 11- 90 cc soda, 50% (50 cc water and 50 cc soda) is poured calmly at the sieve above left hand of the device. 12- Then, turn flare on and sold-water faucet should be opened 13- As long as volume of recipient Erlenmeyer flask is reached approx. 200 cc, flare should be extinguished. 14- Erlenmeyer flask with normal 1% soda is highlighted, aimed at distinguishing blue color.
Azotes for 100 gr. sample saffron based on dry substance Measuring mass percentage of raw fiber based on dry substance 1- Weigh amount of 2 to 3 gr. of sample with the precision of 001% gr. and then, pour it inside one-lit. Erlenmeyer flask. 2- 200 ml curry solution of sulfuric acid is added through the application of dispenser, aimed at reaching it to boiling point. 3- 2 or 3 drops of anti-fizzy substance is added to the solution. Connect Erlenmeyer Flask to aerial coolant and boil solution with electric stove within 2 minutes. Let it be boiled for a period of 30 minutes. Sometime, mix it for turning sample particles pasted to the surface inside Erlenmeyer Flask. 4- Prepare Boehner Erlenmeyer with a hurtleshape along with free-ash strainer paper. 5- At the time of boiling, strain digested substances with the help of strainer paper, hot water and sieve through mild suck. Straining operation should be completed within 10 minutes. 6- Wash Erlen Flask in two parts, (with 50 ml boiling water), and pour it in a sieve equipped with strainer. 7- Wash insolvent substance on straining paper in a one liter balloon through the application of dispenser and through the application of 200 ml sodium solution, 8- Add 2 or 3 drops of anti-foaming substance to Erlen Flask and let it be boiled for a period of 30 minutes. 9- Transfer all insolvent materials with the help of pipe connection or using calm sucker to phial crucible connected to Boehner sieve through the application of boiling water. 10- Wash obtained sedimentation with 50 ml boiling water and HCL solution. Eventually, wash remaining sediment two times with ethanol and three times with acetone. 11- Heat crucible and remnants inside it and put in oven at the temperature of 103 degrees of Celsius for a period of two hours. Cool it in desiccators and then weigh it with 0.001 gr. precision. Repeat the operation as long as disparity between two continuous weighs is not exceeded 0.001 gr. Note: This is an admissible alternative. It is preferred to heat its ash rapidly and register the amount of mass (m1) - 12- Put crucible and sediment inside it in furnace at temperature of 550 degrees of Celsius for a period of one hour and let it be cooled in desiccators. Weigh it with 0.001 gr. precision. M0: Weight of tested substance based on gr. M2: mass of crucible and remaining sediment after drying based on gr. |
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