EUROPEAN PHARMACOPOEIA 11.

0 Maize starch

Solubility : practically insoluble in water and in ethanol (96 per 01/2014:0344

cent), miscible with light petroleum (bp : 40-60 °C) and with corrected 11.0
methylene chloride.
Relative density : about 0.920.
Refractive index : about 1.474.

MAIZE STARCH(2)
IDENTIFICATION
First identification : B. Maydis amylum
Second identification : A.
DEFINITION
A. Identification of fatty oils by thin-layer chromatography
(2.3.2). Maize starch is obtained from the caryopsis of Zea mays L.

is similar to the chromatogram obtained with the reference ♦CHARACTERS

Results : the chromatogram obtained with the test solution

solution. Appearance : matt, white to slightly yellowish, very fine powder

that creaks when pressed between the fingers.
B. Composition of fatty acids (see Tests).
Solubility : practically insoluble in cold water and in ethanol
(96 per cent).
TESTS
The presence of granules with cracks or irregularities on the
Acid value (2.5.1): maximum 0.5, or maximum 0.3 if intended edge is exceptional.♦
for use in the manufacture of parenteral preparations,
determined on 10.0 g.
IDENTIFICATION
Peroxide value (2.5.5, Method A) : maximum 10.0, or
A. Microscopic examination (2.8.23), using a 50 per cent V/V
maximum 5.0 if intended for use in the manufacture of
solution of glycerol R. It appears as either angular polyhedral
parenteral preparations.
granules of irregular sizes with diameters ranging from
Unsaponifiable matter (2.5.7): maximum 2.8 per cent, about 2 μm to about 23 μm or as rounded or spheroidal
determined on 5.0 g. granules of irregular sizes with diameters ranging from
Alkaline impurities (2.4.19). It complies with the test. about 25 μm to about 35 μm (Figure 0344.-1). The central
hilum consists of a distinct cavity or 2- to 5-rayed cleft and
Composition of fatty acids (2.4.22, Method A). Use the there are no concentric striations. Between orthogonally
mixture of calibrating substances in Table 2.4.22.-3. orientated polarising plates or prisms, the starch granules
Composition of the fatty-acid fraction of the oil : show a distinct black cross intersecting at the hilum.

– sum of fatty acids of chain length less than C16 : maximum

0.6 per cent ;
– palmitic acid : 8.6 per cent to 16.5 per cent ;
– stearic acid : maximum 3.3 per cent ;
– oleic acid and isomer : 20.0 per cent to 42.2 per cent ;
– linoleic acid : 39.4 per cent to 65.6 per cent ;
– linolenic acid : 0.5 per cent to 1.5 per cent ;
– arachidic acid : maximum 0.8 per cent ;
– eicosenoic acid : maximum 0.5 per cent ;
– behenic acid : maximum 0.5 per cent ;
– any other fatty acid : for each fatty acid, maximum 0.5 per
cent.
Water (2.5.32) : maximum 0.1 per cent, determined on 1.00 g.

STORAGE
Protected from light, at a temperature not exceeding 25 °C.

LABELLING Figure 0344.-1. – Illustration for identification test A of maize

starch
The label states :
B. Suspend 1 g in 50 mL of water R, boil for 1 min and cool.
– where applicable, that the substance is suitable for use in A thin, cloudy mucilage is formed.
the manufacture of parenteral preparations ;
C. To 1 mL of the mucilage obtained in identification test B
– whether the oil is obtained by mechanical expression or add 0.05 mL of iodine solution R1. An orange-red to dark
by extraction. blue colour is produced, which disappears on heating.
(2) This monograph has undergone pharmacopoeial harmonisation. See chapter 5.8. Pharmacopoeial harmonisation.

General Notices (1) apply to all monographs and other texts 3311
Malathion EUROPEAN PHARMACOPOEIA 11.0

TESTS Test solution (a). Dissolve 0.10 g of the substance to be

pH (2.2.3) : 4.0 to 7.0. examined in the solvent mixture and dilute to 5.0 mL with the
solvent mixture.
To 5.0 g add 25.0 mL of carbon dioxide-free water R. Agitate
continuously at a moderate rate for 60 s. Stop the agitation Test solution (b). Dilute 1.0 mL of test solution (a) to 10.0 mL
and allow to stand for 15 min. with the solvent mixture.
◊Foreign matter. Examined under a microscope using a Reference solution (a). Dissolve 0.100 g of malathion CRS in
50 per cent V/V solution of glycerol R, not more than traces the solvent mixture and dilute to 50.0 mL with the solvent
of matter other than starch granules are present. No starch mixture.
granules of any other origin are present.◊ Reference solution (b). Dilute 0.5 mL of test solution (a) to
100.0 mL with the solvent mixture.
Oxidising substances (2.5.30) : maximum 20 ppm, calculated
as H2O2. Reference solution (c). Dissolve 5.0 mg of malathion
impurity A CRS and 5.0 mg of malathion impurity B CRS in
Sulfur dioxide (2.5.29) : maximum 50 ppm. the solvent mixture, then dilute 50.0 mL with the solvent
Iron (2.4.9) : maximum 10 ppm. mixture.
Shake 1.5 g with 15 mL of dilute hydrochloric acid R. Filter. Reference solution (d). Dilute 2.0 mL of reference solution (c)
The filtrate complies with the test. to 10.0 mL with the solvent mixture.
Loss on drying (2.2.32) : maximum 15.0 per cent, determined Column :
on 1.000 g by drying in an oven at 130 °C for 90 min. – size : l = 0.15 m, Ø = 4.6 mm ;
Sulfated ash (2.4.14) : maximum 0.6 per cent, determined on – stationary phase : octadecylsilyl silica gel for
1.0 g. chromatography R (10 μm) ;
Microbial contamination – temperature : 35 °C.
TAMC : acceptance criterion 103 CFU/g (2.6.12). Mobile phase : acetonitrile R, water R (45:55 V/V).
TYMC : acceptance criterion 102 CFU/g (2.6.12). Flow rate : 1 mL/min.
Absence of Escherichia coli (2.6.13). Detection : spectrophotometer at 210 nm.
◊Absence of Salmonella (2.6.13).◊ Injection : 20 μL of test solution (a) and reference solutions (b),
(c) and (d).
01/2008:1343 Retention time : impurity B = about 3.5 min ;
impurity A = about 5 min ; malathion = about 16 min.
System suitability : reference solution (c) :
– resolution : minimum 2.0 between the peaks due to
impurities B and A.
MALATHION Limits :
– impurity A : not more than 3 times the area of the
corresponding peak in the chromatogram obtained with
Malathionum reference solution (d) (0.3 per cent) ;
– impurity B : not more than the area of the corresponding
peak in the chromatogram obtained with reference
solution (d) (0.1 per cent) ;
– sum of impurities other than A and B : not more than
twice the area of the principal peak in the chromatogram
obtained with reference solution (b) (1 per cent) ;
C10H19O6PS2 Mr 330.4 – disregard limit : 0.1 times the area of the principal peak in
[121-75-5] the chromatogram obtained with reference solution (b)
DEFINITION (0.05 per cent).
Diethyl (2RS)-2-(dimethoxyphosphinodithioyl)butanedioate. Water (2.5.12) : maximum 0.1 per cent, determined on 2.000 g.
Content : 98.0 per cent to 102.0 per cent (anhydrous substance). ASSAY
CHARACTERS Liquid chromatography (2.2.29) as described in the test for
Appearance : clear, colourless or slightly yellowish liquid. related substances with the following modifications.
Solubility : slightly soluble in water, miscible with acetone, with Injection : test solution (b) and reference solution (a).
cyclohexane, with ethanol (96 per cent) and with vegetable System suitability : reference solution (a) :
oils. – repeatability : maximum relative standard deviation of
It solidifies at about 3 °C. 1.0 per cent after 6 injections.
Calculate the percentage content of C10H19O6PS2 from the
IDENTIFICATION declared content of malathion CRS.
Infrared absorption spectrophotometry (2.2.24).
Comparison : malathion CRS. STORAGE
In an airtight container, protected from light.
TESTS
Relative density (2.2.5) : 1.220 to 1.240. IMPURITIES
Optical rotation (2.2.7): − 0.1° to + 0.1°. Specified impurities : A, B.
Dissolve 2.50 g in ethanol (96 per cent) R and dilute to 25.0 mL Other detectable impurities (the following substances would,
with the same solvent. if present at a sufficient level, be detected by one or other of
the tests in the monograph. They are limited by the general
Related substances. Liquid chromatography (2.2.29). acceptance criterion for other/unspecified impurities and/or
Solvent mixture : water R, acetonitrile R (1:3 V/V). by the general monograph Substances for pharmaceutical

3312 See the information section on general monographs (cover pages)