甲磺酸伊马替尼含量检测方法

This paper describes the development and validation of a new, simple, fast, and sensitive liquid chromatographic method for the determination of imatinib mesylate. Imatinib mesylate is not listed in any

pharmacopoeia, and there are few methods in the literature for its quantitation in pharmaceutical dosage forms. In this work, a C18

μBondapak® (3.9150 mm, 5 µm) column was used as the stationary phase, and 30 mM sodium heptane sulphonic acid in 0.01 M KH2PO4 (pH 2.5):MeOH (42:58) was the mobile phase. Detection was performed on a UV detector at 237 nm. Through the evaluation of the analytical parameters, it was shown that the method is linear (r=0.9994) at concentrations ranging from 0.3 mg/mL to 0.8 mg/mL. The relative standard deviation values [RSD] for intra- and inter-day precision studies were 1.7 and 2.6. Recoveries ranged between 96.2 and 101.4.

Keywords: Imatinib mesylate; HPLC; Assay; Stability-indicating method

Abstract

The reversed-phase high-performance liquid chromatographic (RP-HPLC) method has been developed and validated for the simultaneous determination of imatinib mesylate and of the impurity product in Glivec capsules (Novartis, Switzerland). Separations were performed on a X Terra 150 mm x 4.6 mm, 5 microm particle size column at 25 degrees C. The mobile phase was a mixture of methanol-water-triethylamine (25:74:1, v/v/v) with flow rate of 1.0 ml min(-1). pH value of water-triethylamine (TEA) was adjusted to 2.4 with orthophosphoric acid before adding of methanol. UV detection was performed at 267 nm. Acetaminophen was used as an internal standard. The method was validated statistically for its selectivity, linearity, precision, accuracy and robustness. Due to its speed and accuracy, the method may be used for quality control analyses.

Abstract

The reversed-phase high-performance liquid chromatographic (RP-HPLC) method has been developed and validated for the simultaneous determination of imatinib mesylate and of the impurity product in Glivec capsules (Novartis, Switzerland). Separations were performed on a X Terra 150 mm x 4.6 mm, 5 microm particle size column at 25 degrees C. The mobile phase was a mixture of methanol-water-triethylamine (25:74:1, v/v/v) with flow rate of 1.0 ml min(-1). pH value of water-triethylamine (TEA) was adjusted to 2.4 with orthophosphoric acid before adding of methanol. UV detection was performed at 267 nm. Acetaminophen was used as an internal standard. The method was validated statistically for its selectivity, linearity, precision, accuracy and robustness. Due to its speed and

accuracy, the method may be used for quality control analyses.

PMID: 14698262 [PubMed - indexed for MEDLINE]