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

Analytica ◽  
2021 ◽  
Vol 2 (4) ◽  
pp. 121-129
Author(s):  
Eleni Doulou ◽  
Marina Kalomiraki ◽  
Anthi Parla ◽  
Kyriaki Thermos ◽  
Nikos A. Chaniotakis ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
High Sensitivity ◽  
Ammonium Bicarbonate ◽  
Hydrophilic Interaction Liquid Chromatography ◽  
Excitation Wavelength ◽  
Hydrophilic Interaction ◽  
Severe Diarrhea ◽  
Sensitivity And Selectivity ◽  
Sample Preparation Procedure

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.

scholarly journals Fast HPLC Method Using Ion-Pair and Hydrophilic Interaction Liquid Chromatography for Determination of Phenylephrine in Pharmaceutical Formulations

2010 ◽  
Vol 93 (5) ◽  
pp. 1436-1442 ◽  
Author(s):  
Michal Douòa ◽  
Petr Gibala
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Ion Pair ◽  
Hydrophilic Interaction Liquid Chromatography ◽  
Hydrophilic Interaction ◽  
Injection Volume ◽  
Ion Pair Chromatography

Abstract A rapid procedure based on a direct extraction and HPLC determination with fluorescence detection of phenylephrine in pharmaceutical sachets that include a large excess of paracetamol (65 + 1, w/w), ascorbic acid (5 + 1, w/w), and other excipients (aspartame and sucrose) was developed and validated. The final optimized chromatographic method for ion-pair chromatography used an XTerra RP18 column, 3 µm particle size, 50 ⨯ 3.0 mm id. The mobile phase consisted of a mixture of acetonitrile and buffer (10 mM sodium octane-1-sulfonate, adjusted with H3PO4 to pH 2.2; 200 + 800, v/v), with a constant flow rate of 0.3 mL/min. The separation was carried out at 30C, and the injection volume was 3 µL. Fluorescence detection was performed at excitation and emission wavelengths of 275 and 310 nm, respectively. The mobile phase parameters, such as the organic solvent fraction (acetonitrile) in mobile phase as an organic modifier, the concentration of sodium octane-1-sulfonate as a counter-ion, temperature, and pH of mobile phase, were studied. As an alternative to ion-pair chromatography, hydrophilic interaction liquid chromatography (HILIC) was investigated using a Luna HILIC column, 3 m, 100 ⨯ 4.6 mm id. The mobile phase consisted of acetonitrile and buffer (5 M potassium dihydrogen phosphate, adjusted with H3PO4 to pH 2.5; 750 + 250, v/v) at a flow rate of 0.8 mL/min. The separation was carried out at 25°C, and the injection volume was 5 µL. The proposed method has an advantage of a very simple sample pretreatment, and is much faster than the currently utilized HPLC methods using gradient elution and UV detection. Commercial samples of sachets were successfully analyzed by the proposed HPLC method.

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