Analysis of chlorpheniramine in human urine samples using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography

Mehdi Maham,Vahid Kiarostami,Malihe Khoeini Sharifabadi,Syed Waqif-Husain

doi:10.1590/s1984-82502014000300014

Abstract

A simple and environmentally friendly microextraction technique was used for determination of chlorpheniramine (CPM), an antihistamine drug, in human urine samples using dispersive liquid-liquid microextraction (DLLME) followed by high performance liquid chromatography with diode array detection (HPLC-DAD). In this extraction technique, an appropriate mixture of acetonitrile (disperser solvent) and carbon tetrachloride (extraction solvent) was rapidly injected into the urine sample containing the target analyte. Tiny droplets of extractant were formed and dispersed into the sample solution and then sedimented at the bottom of the conical test tube by centrifugation. Under optimal conditions, the calibration curve was linear in the range of 0.055-5.5 µg mL-1, with a detection limit of 16.5 ng mL-1. This proposed method was successfully applied to the analysis of real urine samples. Low consumption of toxic organic solvents, simplicity of operation, low cost and acceptable figures of merit are the main advantages of the proposed technique.

Highlights

Chlorpheniramine (CPM, [3-(p-chlorophenyl)-3-(2pyridyl)-N,N-dimethylpropylamine]) is a histamine H1receptor antagonist, which is often found as an ingredient of ‘over-the counter’ treatments to alleviate symptoms of the common cold and allergic conditions (Fried et al, 2002)
In order to obtain maximum extraction efficiency, some important parameters such as extraction solvent type must be investigated in detail
In conventional Dispersive liquid–liquid microextraction (DLLME), the extraction solvent should have a higher density than water to be collected at the bottom of the test tube after centrifuging

Summary

Introduction

Chlorpheniramine (CPM, [3-(p-chlorophenyl)-3-(2pyridyl)-N,N-dimethylpropylamine]) is a histamine H1receptor antagonist, which is often found as an ingredient of ‘over-the counter’ treatments to alleviate symptoms of the common cold and allergic conditions (Fried et al, 2002). Traditional methods such as liquid–liquid extraction (LLE) and solid phase extraction (SPE) have been widely used as sample preparation methods for extraction and preconcentration of analytes (Benjamin, Xiaochen, 2007; Zhu et al, 2011) These methods are time consuming, tedious, relatively expensive and use large amounts of sample and toxic organic solvents and produce high secondary wastes. Dispersive liquid–liquid microextraction (DLLME) has been introduced as a novel LPME by Assadi research group (Rezaee et al, 2006) In the latter technique, a suitable mixture of extraction and disperser solvents is rapidly injected into the aqueous sample by a syringe. Determination of analyte in the sediment phase can be accomplished by instrumental techniques (Ezoddin, Shemirani, Jamali, 2010; Kazemi, Shokoufi, Shemirani, 2011)

Methods

Results

Conclusion