gHK DETERMINATION OP COUMARIN 301 TOBACCO AND ...

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* (d) Meanwhile two chromatography solumns (height 30cm, diameter 1cm, each containing a glass wool plug) are prepared by pouring a Blurry of silicic acid in solvent mixture B to heights of 5.7cm and 8.0cm respectively, (e) The dry organic solution from (o) is filtered by suotion through a Cambridge filter pad into a Buchner flask* The magnesium sulphate residue is washed with two 30ml portions of solvent mixture A, (f) The filtrate (plus washings) is transferred to a 11 round bottomed flask and concentrated to a volume- of less than 50ml and on a rotary evaporator using a water bath at room temperature. (g) The Bolution in the round bottomed flask is quantitatively transferred to a 50ml pear shaped flask. This solution is concentrated to small bulk (approx. 4-5ml) on a rotary exaporator UBing a water bath at room temperature. (h) The concentrated organic solution is quantitatively transferred by Pasteur pipette to the smaller silioic acid column (height 5*7cm). Bie pear shaped flask is rinsed with small quantities (3 x 1ml) of solvent mixture £ and these washings are transferred to the column. (i) The column is eluted with solvent mixture B. The first JOBUB are discarded and the 30-60 ml fraction is collected in a graduated cylinder. (j) The 30-60 ml fraction is transferred to a 50ml pear shaped flask and the solution is evaporated to dryness on a rotary evaporator at room temperature. (k) The residue in the pear shaped flask iB dissolved in a small volume of solvent mixture B (approx. 3 m l)» This is quantitatively transferred by Pasteur pipette to the second silicic acid column (height 8.0cm). The flask is rinsed with small quantities (2 x 1ml) of solvent mixture B«nd the washings are transferred to the column. (l) The column is eluted with solvent mixture B. The first 43ml are discarded and the 4&-75ml fraction is collected in a graduated cylinder. (m) The 48-75ml fraction is transferred to a 50ml pear shaped flask 1 and the solution is evaporated to dryness on a rotary evaporator at room temperature. (n). The residue in the f£ask is dissolved in 2ml dichloromethene (added by a pipette). 2ul of this sample is injected into the gas chromatography The approximate concentration of aoumarin in the sample can be obtained from the calibration graph. A standard of approximately the same coumarin concentration is then injected. The volume of the standard solution injected is chosen to give a coumarin peak of approximately the same height as the Bame peak. http://legacy.library.ucsf.edu/tid/iyl97h00/pdf It is recommended that two sample injections are made i.e. the sequencet sample—> standard—* sample —* standard should be followed.
3* CALCULATION OF RESULT AMOUNT OP COUMARIN IN SMOKE (^g/cig) t mjtoog,, R*» McKeivor 17.5.76 m/xp COUMARIN CONTENT OF = STANDARD SOLUTION (uq/fil) 1 HEIGHT OF COUMARIN PEAK IN SAMPLE HEIGHT OP STANDARD PEAK http://legacy.library.ucsf.edu/tid/iyl97h00/pdf PINAL VOL, OF SAMPLE SOLN. (jul) VOL. OF SAMPLE INJECTED (^Jl) VOL. STANDARD INJECTED {/up NO. OF CIGARETTES SMOKED
Page 1 and 2: COUMARIK IN TOBACCO gHK DETERMINATI
Page 3 and 4: IABLE II COTJMARIN IEVEL IN PARK DR
Page 5 and 6: TIT;...,'"("" ". ; *."•" jt 6± 1
Page 7 and 8: 7* SWMAKY o In view of the low coum
Page 9: Coumarin standard solutions in dich
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gHK DETERMINATION OP COUMARIN 301 TOBACCO AND ...

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