Stability of Oral Oxytocics in Tropical Climates - Results of Simulation Studies on Oral Ergometrine, Oral Methylergometrine, Buccal Oxytocin and Buccal Desamino-Oxytocin - EDM Research Series No. 012
(1994; 52 pages) Ver el documento en el formato PDF
Índice de contenido
Ver el documentoAbbreviations
Ver el documentoSummary
Abrir esta carpeta y ver su contenidoIntroduction
Cerrar esta carpetaMaterials and methods
Ver el documentoDefinitions used in the study
Ver el documentoSimulated tropical conditions
Ver el documentoMaterials
Ver el documentoAssay method
Ver el documentoStatistics
Abrir esta carpeta y ver su contenidoResults
Abrir esta carpeta y ver su contenidoDiscussion
Ver el documentoConclusions and recommendations
Ver el documentoReferences
Abrir esta carpeta y ver su contenidoAnnexes
 

Assay method

Level of active ingredient was measured by High Performance/Pressure Liquid Chromatography (HPLC). This method can differentiate between the active principle and its degradation products. The Radio Immuno Assay, another assay method, is unable to make this distinction. However, this latter method is more sensitive than the HPLC assay (15,21-27).

HPLC-conditions: ergometrine and methylergometrine

Column:

Spherisorb 5 ODS (250*4.6 mm) chrompack (Bergen op Zoom, Netherlands)

Mobile phase:

A = acetonitrile

 

B = 0.067 M KH2SO4: 0.05% diethylamine H2O

 

A = 60%; B = 40%; (1:1)

Wavelength:

UV: 240 nm

Flow:

1.2 ml/min

Injection volume:

100 ml

Retention time:

6.8 min

Reference solutions:

Freshly made before each new set of runs, with increasing concentrations from solution I to IV

Apparatus:

SP8800 ternary HPLC pump, a Spectra Physics UV detector 757 and an SP 4290 integrator (Spectra Physics)

Calibration curves

Ergometrine:

r = 0.9999

 

Methylergometrine:

r = 0.9999

Table III: Inter-day and intra-day coefficients of variation of (methyl)ergometrine in water

Compound

Coefficient of variation (n =4/6) (%)

 

Concentration of free base (mg/tablet)

Inter-day (n=4)

Intra-day (n=6)

Ergometrine

147

1.2

1.73

Methyl- ergometrine

95

2.2

5.07

HPLC-conditions: oxytocin and desamino-oxytocin

Column:

Spherisorb 5.0 ODS(250*4.6mm) chromopack

Mobile phase:

A: acetonitrile/H2O 1:1

 

B: 0.1 M monobasicKH2PO4

 

buffer A = 55% ; B = 45%

Wavelength:

UV: 225 nm

Flow:

1.2 ml/min

Injection volume:

100 ml

Retention time:

6.7 min

Reference solutions:

Freshly made before each new set of runs, with increasing concentrations from solution I to IV.

Apparatus:

SP8800 ternary HPLC pump, a UV detector 757 and an SP 4290 integrator (Spectra Physics).

Calibration curves:

Oxytocin:

r = 0.9999

 

Desamino-oxytocin:

r = 0.9999

Table IV: Inter-day and intra-day coefficients of variation of desamino-oxytocin in water

C Compound

Coefficient of variation (n =4/6) (%)

 

Concentration (IU/tablet)

Inter-day (n=4)

Intra-day (n=6)

Oxytocin

200

1.90

2.06

Desamino- oxytocin

50

3.19

1.96

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Última actualización: le 3 mayo 2013