Determination of residual dimethylaminopropylamine in aminopropylamides of fatty acid using high-performance liquid chromatography

2021 ◽  
Vol 87 (4) ◽  
pp. 21-25
Author(s):  
D. A. Krasnikov ◽  
I. V. Demchak ◽  
E. S. Khudoleeva
Keyword(s):  
Fatty Acids ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Sulfonyl Chloride ◽  
Phosphate Buffer Solution ◽  
Array Detector ◽  
Precolumn Derivatization ◽  
Buffer Solution

A procedure for determination of the residual content of N,N-dimethyl-1,3-propanediamine (DMAPA) during synthesis of N,N-dimethylaminopropylamides of fatty acids (DMAPA FA) from coconut oil has been developed. The analysis was performed using high performance liquid chromatography on a Shimadzu LC-20 Prominence device equipped with a diode array detector and reversed phase column GL Sciences Inertsil ODS-3. Precolumn derivatization was carried out with a 13% — dansyl chloride (5-(dimethylamino)naphthalene-1-sulfonyl chloride) solution in acetone to increase the analyte response. The selected composition of the mobile phase — acetonitrile and triethylamine phosphate buffer solution (pH 3.0) in a volume ratio of 2:3 and optimized chromatographic conditions provided a clear peak of DMAPA with a retention time of 8.7 – 8.9 min. The proposed method provides determination of 0.02 – 10% DMAPA in DMAPAFA samples. Correctness of the procedure was confirmed in spike tests. The results obtained can be used for assessing the degree of conversion of starting materials in the synthesis of N,N-dimethylaminopropylamides of fatty acids, as well as for forecasting the content of N,N-dimethyl-1,3-propanediamine in the products on their base.

scholarly journals A Validated Stability-indicating Reverse Phase HPLC Assay Method for the Determination of Memantine Hydrochloride Drug Substance with UV-Detection Using Precolumn Derivatization Technique

2010 ◽  
Vol 5 ◽  
pp. ACI.S3936 ◽  
Author(s):  
Bhavil Narola ◽  
A.S. Singh ◽  
P. Rita Santhakumar ◽  
T.G. Chandrashekhar
Keyword(s):  
High Performance ◽  
Phosphate Buffer Solution ◽  
Assay Method ◽  
Array Detector ◽  
Forced Degradation ◽  
Precolumn Derivatization ◽  
Borate Buffer Solution ◽  
Buffer Solution ◽  
Stability Indicating

This present paper deals with the development and validation of a stability indicating high performance liquid chromatographic method for the quantitative determination of Memantine hydrochloride. Memantine hydrochloride was derivatized with 0.015 M 9-fluorenylmethyl chloroformate (FMOC) and 0.5 M borate buffer solution by keeping it at room temperature for about 20 minutes and the chromatographic separation achieved by injecting 10 μL of the derivatized mixture into a Waters HPLC system with photodiode array detector using a kromasil C18 column (150 × 4.6 mm), 5 μ, The mobile phase consisting of 80% acetonitrile and 20% phosphate buffer solution and a flow rate of 2 milliliter/minute. The Memantine was eluted at approximately 7.5 minutes. The volume of FMOC used in derivatization, concentration of FMOC and derivatization time was optimized and used. Forced degradation studies were performed on bulk sample of Memantine hydrochloride using acid (5.0 Normal (N) hydrochloric acid), base (1.0 N sodium hydroxide), oxidation (30% hydrogen peroxide), thermal (105°C), photolytic and humidity conditions. The developed LC method was validated with respect to specificity, precision (% RSD about 0.70%), linearity (linearity of range about 70-130 μg/mL), ruggedness (Overall % RSD about 0.35%), stability in analytical solution (Cumulative % RSD about 0.11% after 1450 min.) and robustness.

Simultaneous Determination of Six Components in Jingzhiguanxin Tablet by High-Performance Liquid Chromatography

2019 ◽  
Vol 15 (2) ◽  
pp. 130-137
Author(s):  
Hui Jiang ◽  
Lianhao Fu ◽  
Yu Wang ◽  
Shaozhi Wang ◽  
Xiaoxu Zhang ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Gradient Elution ◽  
Tanshinone Iia ◽  
Array Detector ◽  
Control Analysis ◽  
Active Components ◽  
Quality Control Analysis

Background: Jingzhiguanxin (JZGX) tablet, a traditional Chinese prescription, is commonly used for treating coronary heart disease and angina pectoris in the clinic. There are six active components (Danshensu (DSS), Protocatechuic aldehyde (PD), Paeoniflorin (PF), Ferulic acid (FA), Salvianolic acid B (Sal B) and Tanshinone IIA (TA)) in JZGX tablet. </P><P> Objective: In this paper, a simple and reliable method was used for simultaneous determining the six active components by high-performance liquid chromatography coupled with diode array detector (HPLC-DAD). Methods: These six active components were separated on an Agilent Zorbax Eclipse XDB-C18 column (150 mmx4.6 mm, 5 µm) at 30 °C. Acetonitrile (A), methanol (B) and 0.5% H3PO4 aqueous solution (C) were used as mobile phase for gradient elution. The flow rate was 1 mL/min and the detection wavelengths were set at 280 nm for DSS, PD and Sal B, 230 nm for PF, 320 nm for FA and 270 nm for TA, respectively. Results: All of the six components showed good linearity regressions (r2≥0.9997) in the detected concentration range. The recovery rates and coefficient of variation (CV) for all analytes were 98.66%- 100.18% and 0.75%-1.89%, respectively. This method was successfully applied to simultaneously determine the six components in JZGX tablet from different batches and manufacturers. Conclusion: The validated method can be used in routine quality control analysis of JZGX tablet without any interference.

Establishment of an HPLC Method for Determination of Coumarin-3-Carboxylic Acid Analogues in Rat Plasma and a Preliminary Study on Their Pharmacokinetics

2021 ◽  
Author(s):  
Yan Xiong ◽  
Yong-Hong Liu ◽  
Jian-Sha Li ◽  
Yu-Ying Zhang ◽  
Jing Zhang ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Carboxylic Acid ◽  
High Performance ◽  
Rat Plasma ◽  
Hplc Method ◽  
Array Detector ◽  
Pharmacokinetic Parameters ◽  
Preliminary Study

Abstract A simple high performance liquid chromatography (HPLC) method was developed and validated for the determination of coumarin-3-carboxylic acid analogues (C3AA) in rat plasma and a preliminary study on pharmacokinetics. Ferulic acid (FA) was used as the internal standard substance, and coumarin-3-carboxylic acid (C3A) was used as a substitute for quantitative C3AA. After protein precipitation with methanol, the satisfactory separation was achieved on an ODS2 column when the temperature was maintained at 30 ± 2°C. The correlation coefficient r in the C3A linear equation is equal to 0.9990. Pharmacokinetic parameters for t1/2, Tmax, Cmax, area under the curve (AUC)0-t, average residence time (MRT), apparent volume of distribution (V z/F) and clearance (Cl/F) were 1.89 ± 0.03 h, 0.39 ± 0.14 h, 1.81 ± 0.10 g· mL−1 ·h, 7.88 ± 0.24 g·mL−1·h, 3.23 ± 0.14 h, 0.43 ± 0.03 (mg·kg−1)·(g·mL−1)−1·h−1, respectively. The high performance liquid chromatography-photo diode array detector (HPLC-PDA) method established in this study can be used to separate and determine the content of C3AA in plasma of rats after 60% ethanol extraction by gavage. The plasma concentration-time curve and pharmacokinetic parameters reflect the absorption of C3AA in rat blood after oral administration to some extent.

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