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MINT OIL_ PARTLY DEMENTHOLISED Menthae arvensis aetheroleum partim

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MINT OIL_ PARTLY DEMENTHOLISED Menthae arvensis aetheroleum partim Powered By Docstoc
					Mint oil, partly dementholised                                                               EUROPEAN PHARMACOPOEIA 5.0



Heavy metals (2.4.8). 1.0 g complies with the limit test C for                                                          01/2005:1838
heavy metals (20 ppm). Prepare the standard using 2 ml of
lead standard solution (10 ppm Pb) R.
Loss on drying (2.2.32). Not more than 0.5 per cent,             MINT OIL, PARTLY DEMENTHOLISED
determined on 1.000 g by drying in an oven at 100-105 °C.
Sulphated ash (2.4.14). Not more than 0.1 per cent,                       Menthae arvensis aetheroleum
determined on 1.0 g.
                                                                            partim mentholi privum
ASSAY
Dissolve 0.150 g in 50 ml of anhydrous acetic acid R. Titrate    DEFINITION
with 0.1 M perchloric acid, determining the end-point            Essential oil obtained by steam distillation from the fresh,
potentiometrically (2.2.20). Carry out a blank titration.        flowering aerial parts, recently gathered from Mentha
1 ml of 0.1 M perchloric acid is equivalent to 20.93 mg of       canadensis L. (syn. M. arvensis L. var. glabrata (Benth)
C9H15N5O.                                                        Fern., M. arvensis var. piperascens Malinv. ex Holmes),
                                                                 followed by partial separation of menthol by crystallisation.
STORAGE
Store protected from light.                                      CHARACTERS
IMPURITIES                                                       Appearance : colourless or pale yellow to greenish-yellow
                                                                 liquid with a characteristic odour.

                                                                 IDENTIFICATION
                                                                 First identification : B.
                                                                 Second identification : A.
A. 6-chloropyrimidine-2,4-diamine 3-oxide,                       A. Thin-layer chromatography (2.2.27).
                                                                    Test solution. Dissolve 0.1 ml of the substance to be
                                                                    examined in 1.0 ml of toluene R.
                                                                    Reference solution. Dissolve 4 µl of carvone R, 4 µl of
                                                                    pulegone R, 10 µl of menthyl acetate R, 20 µl of cineole R
                                                                    and 50 mg of menthol R in 5 ml of toluene R.
                                                                    Plate : TLC silica gel F254 plate R.
B. 6-chloropyrimidine-2,4-diamine,
                                                                    Mobile phase : ethyl acetate R, toluene R (5:95 V/V).
                                                                    Application : 10 µl, as bands.
                                                                    Development : over a path of 15 cm.
                                                                    Drying : in air.
                                                                    Detection A : examine in ultraviolet light at 254 nm.
                                                                    Results A : see below the sequence of the zones present in
                                                                    the chromatograms obtained with the reference solution
C. 3-(cyanoimino)-3-(piperidin-1-yl)propanamide,                    and the test solution. Furthermore, a quenching zone
                                                                    may be present in the upper third of the chromatogram
                                                                    obtained with the test solution.

                                                                                                Top of the plate
                                                                     Carvone and pulegone : a            A quenching zone
                                                                     quenching zone
                                                                                                         A quenching zone
                                                                           Reference solution                      Test solution
D. 6-[[(4-methylphenyl)sulphonyl]oxy]pyrimidine-2,4-diamine
   3-oxide,                                                         Detection B : spray with anisaldehyde solution R and
                                                                    heat at 100-105 °C for 5-10 min. Examine immediately
                                                                    in daylight.
                                                                    Results B : see below the sequence of the zones present
                                                                    in the chromatograms obtained with the reference
                                                                    solution and the test solution. Furthermore, the zone
                                                                    due to cineole in the reference solution is absent in
                                                                    the chromatogram obtained with the test solution. No
                                                                    yellowish-brown zone below the intense reddish-violet
                                                                    zone is present in the chromatogram obtained with the
E. 6-(piperidin-1-yl)pyrimidine-2,4-diamine (desoxyminoxidil).      test solution.


2050                                                     See the information section on general monographs (cover pages)
EUROPEAN PHARMACOPOEIA 5.0                                                                                                      Mitomycin



                                 Top of the plate                          Elution order : order indicated in the composition of the
                                          An intense reddish-violet zone
                                                                           reference solution. Record the retention times of these
                                          (near the solvent front)         substances.
    Menthyl acetate : a bluish-violet     A bluish-violet zone (menthyl    System suitability : reference solution :
    zone                                  acetate)                         — resolution : minimum 1.5 between the peaks due to
                                          A strongly greenish zone             limonene and cineole.
                                          A greenish zone                  Using the retention times determined from the chromatogram
                                                                           obtained with the reference solution, locate the components
    Carvone and pulegone : a reddish      A reddish zone
    zone
                                                                           of the reference solution in the chromatogram obtained with
                                                                           the test solution.
    Cineole : a violet zone
                                                                           Determine the percentage content of these components. The
                                                                           percentages are within the following ranges :
                                          A distinctly violet zone         — limonene : 1.5 per cent to 7.0 per cent,
    Menthol: an intense blue zone         A very intense blue zone         — cineole : maximum 1.5 per cent,
                                          (menthol)                        — menthone : 17.0 per cent to 35.0 per cent,
            Reference solution                      Test solution          — isomenthone : 5.0 per cent to 13.0 per cent,
B. Examine the chromatograms obtained in the test for                      — menthyl acetate : 1.5 per cent to 7.0 per cent,
   chromatographic profile.                                                — isopulegol : 1.0 per cent to 3.0 per cent,
   Results : the characteristic peaks in the chromatogram                  — menthol: 30.0 per cent to 50.0 per cent,
   obtained with the test solution are approximately similar               — pulegone : maximum 2.0 per cent,
   in retention time to those in the chromatogram obtained                 — carvone : maximum 2.0 per cent.
   with the reference solution. Carvone may be absent from
   the chromatogram obtained with the test solution.                       The ratio of cineole content to limonene content is less
                                                                           than 1.
TESTS
                                                                           STORAGE
Relative density (2.2.5) : 0.888 to 0.910.
                                                                           In a well-filled, airtight container, protected from light, at a
Refractive index (2.2.6) : 1.456 to 1.470.                                 temperature not exceeding 25 °C.
Optical rotation (2.2.7) : − 16.0° to − 34.0°.
Acid value (2.5.1) : maximum 1.0, determined on 5.00 g                                                                     01/2005:1655
of the substance to be examined dissolved in 50 ml of the
prescribed mixture of solvents.
                                                                                                 MITOMYCIN
Chromatographic profile. Gas chromatography (2.2.28) :
use the normalisation procedure.                                                                 Mitomycinum
Test solution. Dissolve 0.20 g of the substance to be
examined in hexane R and dilute to 10.0 ml with the same
solvent.
Reference solution. Dissolve 10 mg of limonene R, 20 mg of
cineole R, 40 mg of menthone R, 10 mg of isomenthone R,
40 mg of menthyl acetate R, 20 mg of isopulegol R, 60 mg
of menthol R, 20 mg of pulegone R and 10 mg of carvone R
in hexane R and dilute to 10.0 ml with the same solvent.
Column :
— material : fused silica,
— size : l = 30 m (a film thickness of 1 µm may be used)
    to 60 m (a film thickness of 0.2 µm may be used),                      C15H18N4O5                                              Mr 334.3
    Ø = 0.25-0.53 mm,                                                      DEFINITION
— stationary phase: macrogol 20 000 R.                                     [(1aS,8S,8aR,8bS)-6-Amino-8a-methoxy-5-methyl-4,7-dioxo-
Carrier gas : helium for chromatography R.                                 1,1a,2,4,7,8,8a,8b-octahydroazirino[2′,3′:3,4]pyrrolo[1,2-a]-
Flow rate : 1.5 ml/min.                                                    indol-8-yl]methyl carbamate (mitomycin C).
Split ratio : 1:100.                                                       Substance produced by a strain of Streptomyces caespitotus.
Temperature :                                                              Content : 97.0 per cent to 102.0 per cent (anhydrous
                                                                           substance).
                              Time                  Temperature
                              (min)                    (°C)                CHARACTERS
 Column                       0 - 10                       60              Appearance : blue-violet crystals or crystalline powder.
                              10 - 70                 60 → 180             Solubility : slightly soluble in water, freely soluble in
                                                                           dimethylacetamide, sparingly soluble in methanol, slightly
                              70 - 75                    180
                                                                           soluble in acetone.
 Injection port                                          200
                                                                           IDENTIFICATION
 Detector                                                220
                                                                           A. Infrared absorption spectrophotometry (2.2.24).
Detection : flame ionisation.                                                 Comparison : mitomycin CRS.
Injection : 1.0 µl.                                                        B. Examine the chromatograms obtained in the assay.


General Notices (1) apply to all monographs and other texts                                                                            2051

				
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