Hydrophilic Interaction Liquid Chromatography Coupled with Fluorescence Detection (HILIC-FL) for the Quantitation of Octreotide in Injection Forms

Abstract

Octreotide is a synthetic cyclic octapeptide analogue of somatostatin-14. It is mainly administered for the treatment of acromegaly, severe diarrhea, and neuroendocrine neoplasias. In this work, a hydrophilic interaction liquid chromatography (HILIC) method with fluorescence (FL) detection was developed and validated for the quantitation of octreotide in solutions for injection. Chromatographic separation was performed on an XBridge®-HILIC analytical column under isocratic elution with a short chromatographic run time of less than 10 min. The mobile phase consisted of ammonium bicarbonate 8.6 mM (pH 8.1)/acetonitrile 35/65 (v/v). The high sensitivity and selectivity of the fluorescence detection, with the excitation wavelength (λexcitation) set at 280 nm and the emission wavelength set at (λemission) 330 nm, enabled a simple sample preparation procedure that included only dilution steps. The calibration curve showed good linearity with a correlation coefficient greater than 0.998. The method was successfully applied to the analysis of commercially available octreotide injection forms.

Facile spectrofluorimetric quantitation of octreotide, a synthetic peptide, in its pure form and pharmaceutical formulation; evaluation of the method’s greenness

“…It has been reported that octreotide undergoes disulfide bond cleavage (ringopened form) upon treating with either HCl or NaOH. [12,24,25] This may lead to a significant decrease in the native fluorescence of octreotide. The suggested mechanism for octreotide hydrolysis with HCl and NaOH is shown in Figure 4.…”

“…[4][5][6][7][8] There are not a large number of analytical methods for determining octreotide in its pure form and pharmaceutical formulation. These methods include high-performance liquid chromatography, [9][10][11] liquid chromatography, [12][13][14] electrophoresis, [15] proton ( 1 H) quantitative nuclear magnetic resonance, [16] spectrofluorimetry, [17] and voltammetry. [18] Generally, direct spectrofluorimetric methods based primarily on the measurement of the native drug fluorescence are of great interest.…”

“…There are not a large number of analytical methods for determining octreotide in its pure form and pharmaceutical formulation. These methods include high‐performance liquid chromatography, [ 9–11 ] liquid chromatography, [ 12–14 ] electrophoresis, [ 15 ] proton ( 1 H) quantitative nuclear magnetic resonance, [ 16 ] spectrofluorimetry, [ 17 ] and voltammetry. [ 18 ]…”

HPLC-MS/MS method development and validation for the determination of tetradecapeptide in human plasma

“…Ввиду гидрофильности не для всех соединений возможно подобрать оптимальные условия хроматографического разделения в обращенно-фазовом варианте ВЭЖХ. Альтернативой может стать применение жидкостной хроматографии гидрофильных взаимодействий [hydrophilic interaction liquid chromatography, HILIC] [21,22] либо дериватизация пептида с целью увеличения его липофильности [23]. Кроме того, за счет дериватизации может быть достигнута большая чувствительность при детектировании [23].…”