A Simple, Isocratic and Ultra-Fast Liquid Chromatography / Mass Spectrometry Method for the Estimation of Barnidipine in Human Plasma

Napa Delhiraj Sockalingam
2015 Pharmaceutica Analytica Acta  
An Ultra Fast liquid chromatography -mass spectrometry method (UFLC-MS), for detection and quantification of the anti-hypertensive drug, Barnidipine in human plasma was developed. The Detection was performed using Shimadzu LCMS -2010 EV mass spectrometer with Atmospheric pressure chemical ionization source in negative polarity. Indapamide was used as an internal standard. Selective ion monitoring (SIM) mode was selected with Barnidipine m/z 491 in negative ion mode. Chromatographic separation
more » ... analyte and internal standard were carried out using a reverse phase column, Phenomenex C 18 (50 x 4.6 mm i.d., 5 µ) at a flow rate of 0.300 mL/min. Mobile Phase is composed of Acetonitrile: 0.05 % Formic acid (60:40) v/v. Extracted by Solid Phase Extraction with a sample volume of 200 μL plasma. The assay of Barnidipine is linear over the range of 50 ng/mL to 1000 ng/mL with a precision of <9.86%. Mean extraction recovery for Barnidipine was more than 61%. Samples are stable at room temperature for 6 hrs, processed samples were stable at least for 28 hrs and also stable at three freeze-thaw cycles. The limits of quantification and detection were achieved upto 10 ng/ml and 5 ng/ml respectively. This method was applied successfully to determine Barnipine in plasma samples. was added. The cartridge was washed with 1.0 ml of methanol:water (35:65). The drug and internal standard was eluted from the cartridge using Acetonitrile. The Resulting Solution was used for the analysis. Method validation [5] Linearity: The different concentrations of standard solutions were prepared to contain 50.0 -1000.0 ng/ml of Barnidipine containing 100.00 µg/ml of internal standard. These solutions were analysed and the peak areas and response factors were calculated. The calibration curve was plotted using response factor vs. concentration of the standard solutions. Linear regression analysis (linear equation y = mX + C) of calibration data was applied to calculate the slope (m), intercept (c) and correlation coefficient (r > 0.999).
doi:10.4172/2153-2435.1000400 fatcat:xzz2j6cj5fdq5aifrrkgcrsru4