Journal of AOAC International · 2021
Separation and Determination of Diflunisal and its Impurity by Two Chromatographic Methods: TLC-Densitometry and HPLC.
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Farid Nehal F, Naguib Ibrahim A, Moatamed Radwa S, El Ghobashy Mohamed R
Аннотация
BACKGROUND: Diflunisal (DIF) has analgesic and anti-inflammatory activity. It is a pharmacopeial drug found in the British Pharmacopoeia (BP), and its major pharmacopeial impurity is biphenyl-4-ol (BPL).
OBJECTIVE: DIF has not previously been determined together with BPL. The presence of BPL could significantly affect the dose of DIF in its dosage forms; hence it is crucial to determine DIF and BPL in each other's presence.
METHODS: TLC is the first proposed method, where DIF and BPL were separated on silica gel TLC F254 plates. The eluent was toluene-acetone-acetic acid solution (3.5:6.5:1, v/v). Reversed-phase (RP) HPLC is the second suggested method, where a mixture of DIF and BPL was separated on a C18 (5 µm ps, 250 mm and 4.6 id) column using phosphate buffer pH 4 (0.05 M)-acetonitrile (40:60, v/v). Detection was carried out at 254 nm in both methods.
RESULTS: For the TLC method, concentration ranges of 0.5-3 and 0.3-1.7 µg/band were used, with mean percentage recoveries of 100.22% (SD 0.893) and 100.52% (SD 0.952) for DIF and BPL, respectively. The RP-HPLC method was carried out over a concentration range of 5-30 and 2-9 μg/mL, with mean percentage recoveries of 100.10% (SD 1.259) and 98.88% (SD 0.822) for DIF and BPL, respectively.
CONCLUSION: The TLC and RP-HPLC methods were successfully applied for the determination of DIF and BPL, quantitatively, whether in bulk powder or in pharmaceutical formulations.
HIGHLIGHTS: Two chromatographic methods were developed and validated according to International Council on Harmonization guidelines for the assay of DIF and its pharmacopeial impurity.
OBJECTIVE: DIF has not previously been determined together with BPL. The presence of BPL could significantly affect the dose of DIF in its dosage forms; hence it is crucial to determine DIF and BPL in each other's presence.
METHODS: TLC is the first proposed method, where DIF and BPL were separated on silica gel TLC F254 plates. The eluent was toluene-acetone-acetic acid solution (3.5:6.5:1, v/v). Reversed-phase (RP) HPLC is the second suggested method, where a mixture of DIF and BPL was separated on a C18 (5 µm ps, 250 mm and 4.6 id) column using phosphate buffer pH 4 (0.05 M)-acetonitrile (40:60, v/v). Detection was carried out at 254 nm in both methods.
RESULTS: For the TLC method, concentration ranges of 0.5-3 and 0.3-1.7 µg/band were used, with mean percentage recoveries of 100.22% (SD 0.893) and 100.52% (SD 0.952) for DIF and BPL, respectively. The RP-HPLC method was carried out over a concentration range of 5-30 and 2-9 μg/mL, with mean percentage recoveries of 100.10% (SD 1.259) and 98.88% (SD 0.822) for DIF and BPL, respectively.
CONCLUSION: The TLC and RP-HPLC methods were successfully applied for the determination of DIF and BPL, quantitatively, whether in bulk powder or in pharmaceutical formulations.
HIGHLIGHTS: Two chromatographic methods were developed and validated according to International Council on Harmonization guidelines for the assay of DIF and its pharmacopeial impurity.