36.3.
11 10 mL of this solution with aldehyde-free alcohol to 100 mL in volu-
AOAC Official Method 906.02
Aldehydes (Total)
in Lemon, Orange, and Lime Extracts
Colorimetric Method
First Action 1906
Final Action
A. Reagents
(a) Aldehyde-free alcohol.—Let alcohol, containing 5 g
m-phenylenediamine⋅2HCl/L, stand ≥24 h with frequent shaking.
(Nothing is gained by previous treatment with KOH.) Reflux at least
8 h, longer if necessary; let stand overnight, and distil, rejecting first
10 and last 5 mL distillate. Store in dark, cool place in well filled bot-
tles. (25 mL of this alcohol, on standing 20 min at 14–16°C with
20 mL of the fuchsin-bisulfite solution, should develop only faint
pink tinge. If stronger color develops, repeat above
m-phenylenediamine treatment.) (Avoid skin and eye contact and
breathing m-phenylenediamine dust.)
(b) Fuchsin–bisulfite solution.—Dissolve 0.5 g fuchsin in
250 mL H2O, add aqueous solution containing 16 g SO2, let stand
until colorless or nearly so, and dilute to 1 L with H2O. Let stand 12 h
before use and keep in refrigerator. (This solution may deteriorate
and should be reasonably fresh when used.)
(c) Citral standard solution.—1 mg/mL. Weigh 0.5 g citral into
50 mL volumetric flask, dilute to volume with aldehyde-free alcohol
at room temperature, stopper flask, and mix by shaking. Dilute
metric flask, stopper, and mix.
B. Determination
Weigh ca 25 g extract in stoppered weighing flask, transfer to
50 mL volumetric flask, and dilute to volume at room temperature
with aldehyde-free alcohol. Measure, at room temperature, 2 mL (or
other suitable volume) of this solution into comparison tube. Add
25 mL aldehyde-free alcohol (previously cooled to 14–16°C), then
20 mL fuchsin-bisulfite solution (also cooled), and dilute to 50 mL
with aldehyde-free alcohol. Mix thoroughly, stopper, and keep
15 min at 14–16°C.
Prepare standard for comparison at same time and in same man-
ner, using 2 mL standard citral solution, and compare colors devel-
oped. Calculate amount of citral present and repeat determination,
using amount sufficient to give test portion ca strength of the stan-
dard. From this result calculate amount of citral in extract. If com-
parisons are made in Nessler tubes, standards containing 1, 1.5, 2,
2.5, 3, 3.5, and 4 mg citral may be prepared and trial comparison
made against these, final comparison being made with standards ly-
ing between 1.5 and 2.5 mg with 0.25 mg increments.
It is absolutely essential to keep reagents and comparison tubes at
required temperature, 14–16°C. If comparisons are made in a bath
(possible only when bath is of glass), use standards within 25 min af-
ter adding fuchsin-bisulfite solution. Treat samples and standards
identically.
Reference: J. Am. Chem. Soc. 28, 1472(1906).
© 2000 AOAC INTERNATIONAL