تحديد الميتوكسالين في المستحضرات الصيدلانية باستخدام الاستشراب الغازي الشعري

Abstract EN

An analytical method based on capillary gas chromatography with flame ionization detector (GC–FID) was developed for the direct analysis of Methoxsalen (8-MOP) without derivative reaction, in pure and pharmaceutical dosage forms using Caffeine as internal standard.

The 8-MOP and Caffeine (IS) were dissolved in chloroform and chromatographed on a TRB-5 column (30m×0.25 mm, 0.25 μm), the temperature of GC oven was as follows: initial temperature was 130°C, held for 1 min, increased to 230°C at 20°C/min,and held for 5 min, and then increased to 250°C at 10°C/min with a final hold of 2 min., with nitrogen as carrier gas with flow rate 3 mL/min and FID detection.

The injector port temperature was maintained at 280°C, with split ratio 1:100, and detector temperature was maintained at 300°C.

The method had a chromatographic total run time of 12 min.

The retention times were about 6.8 and 5.7 min for 8-MOP and IS, respectively.

Results of assay and recovery studies were statistically evaluated for its accuracy and precision.

The calibration graph of peak area ratio was rectilinear in the concentration range 10 - 400 μg/mL of 8-MOP, with a relative standard deviation not exceeds 2.12%.

The limit of detection was 1.5μg/mL, and the limit of quantitation was 5 μg/mL.

Correlation coefficient (R2) of the regression equation was greater thane 0.999.

No interference from any components of pharmaceutical dosage forms was observed.