scholarly journals Development and Validation of a Stability-Indicating High-Performance Liquid Chromatography Method for the Simultaneous Determination of Albuterol, Budesonide, and Ipratropium Bromide in Compounded Nebulizer Solutions

2011 ◽  
Vol 94 (1) ◽  
pp. 110-117 ◽  
Author(s):  
Anthony J Blewett ◽  
Deepti Varma ◽  
Tiffany Gilles ◽  
Rashidi Butcher ◽  
Jaini Jacob ◽  
...  
Keyword(s):  
High Performance ◽  
Ipratropium Bromide ◽  
Gradient Elution ◽  
Chromatography Method ◽  
Alkali Solutions ◽  
Ensure Patient Safety ◽  
Liquid Chromatography Method ◽  
Development And Validation ◽  
Hydrolysis Of

Abstract In recent years, there has been a large increase in the use of pharmaceutical compounding to prepare medications that are not commercially available. The treatment of asthma typically includes the use of albuterol (ALB), ipratropium bromide (IPB), and/or budesonide (BUD) nebulizer solutions. There is currently no commercially available nebulizer solution containing all three of these compounds, and patients must rely on often-unregulated compounding. There is a distinct need for methodologies that can be used to analyze compounded formulations to ensure patient safety. We report an HPLC-UV method to separate and quantitate ALB, IPB, and BUD in nebulizer solutions. The method used a gradient elution to achieve separation via an RP C18 column. The method was validated, showed good selectivity, and was linear over several orders of magnitude. The method was applied to the analysis of nebulizer solutions and determination of their storage stability. Significant ALB-dependent degradation occurred within 5 h in solutions formulated with the free base of ALB, while those containing the sulfate salt of ALB produced no degradation. Alkali solutions can cause base-catalyzed hydrolysis of IPB and degradation of BUD. Compounded formulations containing ALB need to include an acid to control pH and prevent degradation.

scholarly journals Development and Validation of an UHPLC-QqQ-MS Technique for Simultaneous Determination of Ten Bioactive Components in Fangji Huangqi Tang

2016 ◽  
Vol 2016 ◽  
pp. 1-8 ◽  
Author(s):  
Xiaoli Wang ◽  
Xiao Liu ◽  
Tingting Zhu ◽  
Baochang Cai
Keyword(s):  
Simultaneous Determination ◽  
Gradient Elution ◽  
Chromatography Method ◽  
Atractylenolide I ◽  
Ultrahigh Performance Liquid Chromatography ◽  
Liquid Chromatography Method ◽  
Development And Validation ◽  
Accuracy And Repeatability ◽  
Atractylenolide Iii

The aim of this study is to develop an ultrahigh performance liquid chromatography method coupled with triple quadrupole mass spectrometry for simultaneous determination of tetrandrine, fangchinoline, atractylenolide I, atractylenolide III, calycosin-7-O-β-D-glucoside, glycyrrhizin, liquiritin, isoliquiritin, liquiritigenin, and isoliquiritigenin in Fangji Huangqi Tang (FHT). The chromatographic separation was performed on a reversed-C18column, eluted with a mixture of 0.1% acetic acid and acetonitrile at 0.4 mL/min. The separation of these ten compounds was achieved by linear gradient elution. The method was strictly validated with respect to specificity, precision, accuracy, and repeatability. All the compounds showed good linearities (r≥0.999). The LOQs of the ten components were 0.36, 0.18, 0.09, 0.43, 0.02, 1.89, 0.26, 0.18, 0.61, and 0.48 ng/mL for tetrandrine, fangchinoline, atractylenolide I, atractylenolide III, calycosin-7-O-β-D-glucoside, glycyrrhizin, liquiritin, isoliquiritin, liquiritigenin, and isoliquiritigenin, respectively. The LODs of the ten components were 0.11, 0.05, 0.03, 0.13, 0.01, 0.57, 0.08, 0.05, 0.18, and 0.14 ng/mL for tetrandrine, fangchinoline, atractylenolide I, atractylenolide III, calycosin-7-O-β-D-glucoside, glycyrrhizin, liquiritin, isoliquiritin, liquiritigenin, and isoliquiritigenin, respectively. The method was proven to be specific and reliable, which would provide a meaningful basis for the quality control and evaluation of FHT during its clinical application.

scholarly journals Development and Validation of a HPLC-UV Method with Pre-column Derivatization for Determination of Cinnabar in Jufang Zhibao Pills

2017 ◽  
Vol 5 (02) ◽  
pp. 01-09
Author(s):  
Xin Zhang ◽  
Jia Yao ◽  
Ying Ren ◽  
Yuan Li ◽  
Zhimin Xie
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
High Accuracy ◽  
Chromatography Method ◽  
Average Recovery ◽  
Sem Image ◽  
Good Repeatability ◽  
Liquid Chromatography Method ◽  
Development And Validation

In this work, a reliable and accurate high-performance liquid chromatography method with pre-column derivatization was established and validated for determination of cinnabar in Jufang Zhibao pills. Scanning electron microscope (SEM) image was used to identify the types of cinnabar crude drug in Jufang Zhibao pills. The chromatography separation was performed on a Welch XB-C18 column (250 mm × 4.6 mm, 5 μm). The mobile phase consists of water spiked with 0.022 mmol/L sodium diethyldithiocarbamate (A, pH adjusted to 8–9 by ammonia water) and methanol (B, 80:20, v/v) at flow rate of 1.0 ml/min with the detected wavelength was 272 nm. The oven temperature was set at 35°C. The calibration for cinnabar content has good linearity (R2 =0.9999) over the range of 2.43–300 μg/ml and the average recovery was less then 1.90%. The limits of detection and quantification were 0.1127 μg and 0.2065 μg/ml. The results indicated that the proposed method has advantages of high accuracy, good repeatability and stability and can be successfully used for determination of cinnabar in Jufang Zhibao pills. It provides a basis for drug manufacture quality control and proves the feasibility of the pre-column derivatization method during the determination of cinnabar in Jufang Zhibao pills.

scholarly journals Determination of Chlorotetracycline and Doxycycline in Medicated Feedingstuffs by Liquid Chromatography

2012 ◽  
Vol 56 (3) ◽  
pp. 329-333 ◽  
Author(s):  
Ewelina Patyra ◽  
Ewelina Kowalczyk ◽  
Krzysztof Kwiatek
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Analytical Procedure ◽  
Solid Phase ◽  
Gradient Elution ◽  
Diode Array ◽  
Chromatography Method ◽  
Array Detection ◽  
Liquid Chromatography Method

Abstract High performance liquid chromatography method with diode array detection (HPLC-DAD) was developed and optimised for the determination of tetracyclines (TCs) in medicated feedingstuffs. The extraction of the analyte from feedingstuffs was performed with Na2EDTA-McIlvaine buffer (pH 2.5 and pH 4). The extracts were cleaned up by solid phase extraction using octadecyl cartridges (C18). The samples were dried up and redissolved in the mixture of oxalic acid and methanol. Separation was performed on reserved phase column (Phenomenex C18, 250 x 4.6 mm, 5 μm) by multistep gradient elution, which provided better chromatographic separation. The analysis was performed at a wavelength of 390 nm. Validation study of the method revealed that all obtained calibration curves showed good linearity R= 0.9985 for doxycycline (DC) and R= 0.9981 for chlorotetracycline (CTC) over the range of 25-2,000 mg/kg. The analytical procedure was successfully adapted for quantitative determination of DC and CTC in medicated feedingstuff samples. Validation included determination of specificity, linearity, and repeatability. Mean recovery for spiked samples was 93.1% for CTC and 93.2% for DC. The results of validation of the analytical procedure proved that presented method is efficient, precise and useful for quantification of DC and CTC in medicated feedingstuffs.

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