Maize oil, refined

EUROPEAN PHARMACOPOEIA 5.0

acid R and 2 ml of barium chloride solution R1. Incinerate

the filter and its contents in a platinum crucible, then ignite
the residue (SiO2) at 900 C to constant mass.

STORAGE
Store protected from light, at a temperature not exceeding
25 C.

01/2005:1342 LABELLING
The label states :
MAIZE OIL, REFINED
where applicable, that the substance is suitable for use in
the manufacture of parenteral dosage forms,
Maydis oleum raffinatum
whether the oil is obtained by mechanical expression or
by extraction.
DEFINITION
Refined maize oil is the fatty oil obtained from the seeds of
01/2005:0344
Zea mays L. by expression or by extraction, then refined.
CHARACTERS
MAIZE STARCH
A clear, light yellow or yellow oil, practically insoluble in
water and in alcohol, miscible with light petroleum (bp :
Maydis amylum
40 C to 60 C) and with methylene chloride.
It has a relative density of about 0.920 and a refractive index DEFINITION
of about 1.474.
Maize starch is obtained from the caryopsis of Zea mays L.
IDENTIFICATION
CHARACTERS
A. Carry out the identification of fatty oils by thin-layer
Appearance : matt, white to slightly yellowish, very fine
chromatography (2.3.2). The chromatogram obtained
powder which creaks when pressed between the fingers.
with the test solution is similar to that obtained with the
Solubility : practically insoluble in cold water and in alcohol.
reference solution.
The presence of granules with cracks or irregularities on
B. It complies with the test for composition of fatty acids
the edge is exceptional.
(see Tests).
It is tasteless.
TESTS
Acid value (2.5.1). Not more than 0.5, determined on 10.0 g. IDENTIFICATION
If intended for use in the manufacture of parenteral dosage A. Examined under a microscope, using not less than
20 magnification and using equal volumes of glycerol R
forms, not more than 0.3.
and water R, it appears as either angular polyhedral
Peroxide value (2.5.5). Not more than 10.0. If intended for
granules of irregular sizes with diameters ranging from
use in the manufacture of parenteral dosage forms, not more
about 2 m to about 23 m or as rounded or spheroidal
than 5.0.
granules of irregular sizes with diameters ranging from
Unsaponifiable matter (2.5.7). Not more than 2.8 per cent,
about 25 m to about 35 m. The central hilum consists
determined on 5.0 g.
of a distinct cavity or two-to five-rayed cleft and there
are no concentric striations. Between crossed nicol
Alkaline impurities (2.4.19). It complies with the test for
prisms, the starch granules show a distinct black cross
alkaline impurities in fatty oils.
intersecting at the hilum.
Composition of fatty acids (2.4.22, Method A). The fatty-acid
B. Suspend 1 g in 50 ml of water R, boil for 1 min and cool.
fraction of the oil has the following composition :
A thin, cloudy mucilage is formed.
fatty acids of chain length less than C16 : not more than
C.
To 10 ml of the mucilage obtained in identification test B
0.6 per cent,
add
0.04 ml of iodine solution R1. An orange-red to dark
palmitic acid : 8.6 per cent to 16.5 per cent,
blue colour is produced which disappears on heating.
stearic acid : not more than 3.3 per cent,
TESTS
oleic acid : 20.0 per cent to 42.2 per cent (equivalent
chain length on polyethyleneglycol adipate 18.3),
pH (2.2.3) : 4.0 to 7.0.
linoleic acid : 39.4 per cent to 65.6 per cent (equivalent
Shake 5.0 g with 25.0 ml of carbon dioxide-free water R for
chain length on polyethyleneglycol adipate 18.9),
60 s. Allow to stand for 15 min.
linolenic acid : 0.5 per cent to 1.5 per cent (equivalent
Foreign matter. Examined under a microscope using a
chain length on polyethyleneglycol adipate 19.7),
mixture of equal volumes of glycerol R and water R, not
arachidic acid : not more than 0.8 per cent,
more than traces of matter other than starch granules are
eicosenoic acid : not more than 0.5 per cent (equivalent present. No starch grains of any other origin are present.
chain length on polyethyleneglycol adipate 20.3),
Oxidising substances (2.5.30) : maximum 20 ppm, calculated
behenic acid : not more than 0.5 per cent,
as H2O2.
other fatty acids : not more than 0.5 per cent.
Sulphur dioxide (2.5.29) : maximum 50 ppm.
Sterols. Determined by gas chromatography (2.4.23), the
Iron (2.4.9) : maximum 10 ppm.
sterol fraction of the oil contains not more than 0.3 per cent
Shake 1.5 g with 15 ml of dilute hydrochloric acid R. Filter.
of brassicasterol.
The filtrate complies with the limit test for iron.
Water (2.5.32). If intended for use in the manufacture
Loss on drying (2.2.32) : maximum 15.0 per cent, determined
of parenteral dosage forms, not more than 0.1 per cent,
on 1.000 g by drying in an oven at 130 C for 90 min.
determined on 5.00 g by the micro-determination of water.
Use a mixture of equal volumes of decanol R and anhydrous Sulphated ash (2.4.14) : maximum 0.6 per cent, determined
on 1.0 g.
methanol R as the solvent.
1964

See the information section on general monographs (cover pages)

EUROPEAN PHARMACOPOEIA 5.0

Malathion

Microbial contamination. Total viable aerobic count

(2.6.12) not more than 103 bacteria and 102 fungi per gram,
determined by plate count. It complies with the test for
Escherichia coli (2.6.13).

ASSAY
Examine by liquid chromatography (2.2.29).
Test solution (a). Dissolve 0.10 g of the substance to be
examined in a mixture of 1 volume of water R and 3 volumes
of acetonitrile R and dilute to 5.0 ml with the same mixture
STORAGE
of solvents.
In an airtight container.
Test solution (b). Take 1.0 ml of test solution (a) and dilute to
10.0 ml with a mixture of 1 volume of water R and 3 volumes
of acetonitrile R.
Reference
solution (a). Dissolve 0.100 g of malathion CRS
01/2005:1343
in a mixture of 1 volume of water R and 3 volumes of
acetonitrile R and dilute to 50.0 ml with the same mixture
MALATHION
of solvents.
Reference solution (b). Take 0.5 ml of test solution (a) and
dilute to 100.0 ml with a mixture of 1 volume of water R and
Malathionum
3 volumes of acetonitrile R.
Reference solution (c). Dissolve 5.0 mg of malathion
impurity A CRS and 5.0 mg of malathion impurity B CRS
in a mixture of 1 volume of water R and 3 volumes of
acetonitrile R and dilute to 50.0 ml with the same mixture
of solvents.
Reference solution (d). Take 2.0 ml of reference solution (c)
and dilute to 10.0 ml with a mixture of 1 volume of water R
C10H19O6PS2
Mr 330.4 and 3 volumes of acetonitrile R.
The chromatographic procedure may be carried out using :
DEFINITION
a stainless steel column 0.15 m long and4.6 mm in
Malathion contains not less than 98.0 per cent and not
internal diameter packed with octadecylsilyl silica gel for
more than the equivalent of 102.0 per cent of diethyl
chromatography R (10 m),
(2RS)-2-(dimethoxyphosphinodithioyl)butanedioate,

as
mobile phase at a flow rate of 1 ml/min a mixture of
calculated with reference to the anhydrous substance.
45 volumes of acetonitrile R and 55 volumes of water R,
CHARACTERS
as detector a spectrophotometer set at 210 nm,
A clear, colourless or slightly yellowish liquid, slightly
maintaining the temperature of the column at 35 C.
soluble in water, miscible with alcohol and with acetone,
Inject 20 l of reference solution (b) and 20 l of reference
with cyclohexane and with vegetable oils.
solution (c).
It freezes at about 3 C.
When the chromatograms are recorded in the prescribed
conditions, the retention times are : impurity B about
IDENTIFICATION
3.5 min ; impurity A about 5 min and malathion about 16 min.
Examine by infrared absorption spectrophotometry (2.2.24), Adjust the sensitivity of the system so that the height of the
comparing with the spectrum obtained with malathion CRS. principal peak in the chromatogram obtained with reference
solution (b) is at least 50 per cent of the full scale of the
TESTS
recorder. The test is not valid unless in the chromatogram
obtained with reference solution (c) the resolution between
Relative density (2.2.5) : 1.220 to 1.240.
the peaks corresponding to impurity A and impurity B is at
Optical rotation (2.2.7). Dissolve 2.50 g in alcohol R and
least 2.0. Inject reference solution (a) six times. The assay is
dilute to 25.0 ml with the same solvent. The angle of optical not valid unless the relative standard deviation of the peak
rotation is 0.1 to + 0.1.
area for malathion is at most 1.0 per cent.
Related substances. Examine by liquid chromatography
Inject alternately test solution (b) and reference solution (a).
(2.2.29) as prescribed under Assay.
Calculate the percentage content of malathion.
Inject 20 l of test solution (a) and 20 l of reference
STORAGE
solution (d). In the chromatogram obtained with test
solution (a) : the area of any peak due to impurity A is not
Store in an airtight container, protected from light.
greater than three times the area of the corresponding peak
IMPURITIES
in the chromatogram obtained with reference solution (d)
(0.3 per cent) ; the area of any peak due to impurity B is
not greater than the area of the corresponding peak in the
chromatogram obtained with reference solution (d) (0.1 per
cent) ; the sum of the areas of all the peaks apart from the
principal peak and any peak due to impurity A or impurity B
is not greater than twice the area of the principal peak in the
chromatogram obtained with reference solution (b) (1 per
cent). Disregard any peak with an area less than 0.1 times
A. X = S : diethyl (2RS)-2-[(methoxy)(methylsulphanyl)-Sthat of the area of the principal peak in the chromatogram
phosphinothioyl]butanedioate (isomalathion),
obtained with reference solution (b).
Water (2.5.12). Not more than 0.1 per cent, determined on
B. X = O : diethyl (2RS)-2-(dimethoxy-S-phosphinothioyl)bu2.000 g by the semi-micro determination of water.
tanedioate (maloxon),
General Notices (1) apply to all monographs and other texts

1965