Article

RP-HPLC-UV method development and validation for simultaneous determination of terbutaline sulphate, ambroxol HCl and guaifenesin in pure and dosage forms

Authors:
  • Karnataka Antibiotics and Pharmaceutical Ltd
To read the full-text of this research, you can request a copy directly from the authors.

Abstract

Objective: The objective of the present work was to develop and validate a simple, sensitive, rapid and stable reverse-phase high performance liquid chromatography (RP-HPLC) method for a combination of Terbutaline sulphate (TSL), Ambroxol hydrochloride (AML) and Guaifenesin (GFN). Method: The combination of these drugs was analyzed by using Shimadzu LC 2010 CHT high performance liquid chromatography (HPLC). Successful separation was achieved by isocratic elution on a reverse-phase C18 column (sun fire) (250mm, 4.6mm, 5μ), using a mobile phase consisting of buffer: acetonitrile in the ratio 80: 20 (buffer - 0.1% v/v triethyleamine pH-3.0) followed by 1.0mL/min flow rate. The wavelength of detection was at 220nm. Result: The chromatographic retention times were consistent at 3.0, 10.5 and 13.8minutes for TSL, AML and GFN respectively. For these three compounds, the lower limit of detection was 1.0, 1.25, and 1.5μg/mL and lower limit of quantification was 3.3, 4.1 and 5.0μg/mL respectively. The linearity concentrations established for TSL, AML and GFN were 1.0-7.0, 1.5-7.5 and 4.0-14.0μg/mL respectively. The correlation coefficients for all the drugs were found to be greater than 0.999. The relative standard deviation of inter- and intra-day were less than 2.0%. Conclusion: This method provides a necessary tool for quantification of the selected drugs for their assay. The proposed method is simple, accurate, reproducible and applied successfully to analyze three compounds in pure as well dosage form.

No full-text available

Request Full-text Paper PDF

To read the full-text of this research,
you can request a copy directly from the authors.

... Both Chlor and Phen were evaluated using HPLC [22,23]. The Gly compound was quantified by spectrophotometric method [24], and was evaluated by high performance liquid chromatography [25,26]. The M.H.B compound was electrically estimated [27]. ...
... Three solutions of Tussilet syrup were prepared containing concentrations (15,20,25) µg / ml of Phen, and the results showed high accuracy and Precision, Rec% ranged between 97.0412 -101.6795% and RSD% ranged between 0.0051-0.0091 as shown in Table 6. ...
Conference Paper
This study Includes innovation and validation of RP-HPLC method for determination of the drugs Chlorpheniramine maleate(Chlor) , Phenylphrine HCl(Phen), Glyceryl guaiacolate(Gly), and the additives Methyl paraben )M.H.B),Propyl paraben(P.H.B) and Yellow dye no.6 by using of L11 column( 25cm×4.6mm,5µm) and mobile phase content of Methanol : water 60:40(v/v) containing 300mg Sodium dihydrogen phosphate , 9 ml Solution of Triethylamine hydrochloride, 300mg Sodium lauryl sulfate, and pH 3.5 the detection was at 269 nm. The method successfully applied to determination of all drugs in pure and in pharmaceutical forms. Rec% was between 95.2677-104.0223, RSD% was between 0.00004-0.0140, LOD was between 0.0001-0.0015µg/ml and LOQ was between 0.0003-0.0045 µg/ml.
... Results of AGREE assessment for reported methods and proposed methods.Reported HPLC-DAD(14) Stationary phase: C18 Mobile phase: acetonitrile: methanol: phosphate buffer (20:5:75 v/v) Flow rate: 1.2 mL/min Run time: 12.0 min ...
Article
Full-text available
Guaifenesin (GUA) is determined in dosage forms and plasma using two methods. The spectrofluorimetric technique relies on the measurement of native fluorescence intensity at 302 nm upon excitation wavelength “223 nm”. The method was validated according to ICH and FDA guidelines. A concentration range of 0.1–1.1 μg/mL was used, with limit of detection (LOD) and quantification (LOQ) values 0.03 and 0.08 µg/mL, respectively. This method was used to measure GUA in tablets and plasma, with %recovery of 100.44% ± 0.037 and 101.03% ± 0.751. Furthermore, multivariate chemometric-assisted spectrophotometric methods are used for the determination of GUA, paracetamol (PARA), oxomemazine (OXO), and sodium benzoate (SB) in their lab mixtures. The concentration ranges of 2.0–10.0, 4.0–16.0, 2.0–10.0, and 3.0–10.0 µg/mL for OXO, GUA, PARA, and SB; respectively, were used. LOD and LOQ were 0.33, 0.68, 0.28, and 0.29 µg/mL, and 1.00, 2.06, 0.84, and 0.87 µg/mL for PARA, GUA, OXO, and SB. For the suppository application, the partial least square (PLS) model was used with %recovery 98.49% ± 0.5, 98.51% ± 0.64, 100.21% ± 0.36 & 98.13% ± 0.51, although the multivariate curve resolution alternating least-squares (MCR-ALS) model was used with %recovery 101.39 ± 0.45, 99.19 ± 0.2, 100.24 ± 0.12, and 98.61 ± 0.32 for OXO, GUA, PARA, and SB. Analytical Eco-scale and Analytical Greenness Assessment were used to assess the greenness level of our techniques.
... Conductometric [23], capillary zone electrophoresis [24], high-performance thinlayer chromatography (HPTLC) [25], and fluorescence spectroscopy [26,27] techniques are used for the determination of phenylephrine hydrochloride. Spectrofluorimetry [28], reversed-phase HPLC [29], HPTLC [30], potentiometric titration [31], and cyclic voltammetry [32] techniques are used for the determination of terbutaline sulfate. Different spectrophotometric methods using various reagents were described for the determination of the above drugs, such as silver triangular nanoplates [33], copper-hexacyanoferrate nanoparticles [34], 5-amino-3-H,1,3,4-thiodiazole-2-thione [35], ferric ion [36], and calcon dye [37] were used for the determination of adrenaline. ...
Article
Full-text available
A spectrophotometric method has been developed for the determination of some amine-phenol containing drugs, namely, adrenaline, phenylephrine hydrochloride and terbutaline sulphate. The method is depended on the formation of new products by reaction of the drugs with Gibb's reagent (2,6-dichloroquinone-4-chloroamide , DCQ) reagent in basic borate buffer medium of pH11. The products were measured at 475, 652.5 and 547 nm for above drugs respectively. Beer’s low was obeyed in the range 0.3-9.5, 0.5-17, and 0.5-55 µg/ml with average recovery% of 101.10, 99.13 and 99.78 and relative standard deviation (RSD) ≤ 3.31, respectively. The method was free from excipients interferences, and applied successfully for assay of the studied drugs in their pharmaceutical formulations. The resulting products were found in the ratio of 1:1.
... Because they do not adhere to RP columns very well, strongly polar compounds, such as organic acids and carbohydrates, are not ideal for use in RP HPLC studies. Hydrophilic interaction chromatography (also known as HILIC) is a new approach that researchers are developing to circumvent this issue (Itagimatha et al 2019). ...
Article
Full-text available
Modern chromatography is mostly used for analytical purposes. Modern pharmaceutical and biological analysis uses HPLC. It separates molecules from heterogeneous liquids and characterizes them. Mass spectrometry identifies peptides, proteins, and other compounds after high-performance liquid chromatography. HPLC's flexibility and dependability (pressure-driven liquid support) make it popular. However, fast separation often creates high operating pressure, which stresses HPLC equipment. Thus, core-shell silica microspheres and zirconia packing have been produced recently. Fused-core or superficially porous microspheres have solid cores with porous shells. Despite its low pressure, this device can separate small, large, and intricate molecules. It is effective and fast. UPLC offers greater resolution, sensitivity, and separation times than HPLC; however, it may be less reproducible. Rapid Resolution Liquid Chromatography (RRLC) is more precise and sensitive than HPLC, improving sample analysis quality and quantity. This review will highlight column technology basics and RP-HPLC advances and focuses on the concept of HPLC.
... In the literature, CAR has been analysed by HPLC [5][6][7][8] and spectrophotometry [9][10][11][12][13], GUF has been analysed using HPLC [14][15][16][17][18][19][20][21], spectrophotometric [22][23][24] and electrochemical [25,26] techniques. HPLC [27,28], electrochemical [26] and Spectrophotometry [29,30] techniques have been used to determine OXO. ...
... For the simultaneous determination of ABH, TES and GPN in liquid dosage form, three RP-HPLC methods and only one spectrophotometric method was reported. [2][3][4] UV-vis spectroscopic methods have the advantage of being simple, easy to use, and relatively less expensive when compared to other popular quantitative methods, and have been widely used in quantitative analysis. However, it is difficult to analyze multi-component formulations that exhibit significant overlapping in their absorption spectra when using direct and conventional UV-spectrophotometric methods without any prior separation. ...
... There are number of analytical methods for the analysis of pharmaceutical drugs from different formulations [6][7][8][9][10][11][12][13][14][15][16][17][18][19]. Literature survey revealed various analytical methods have been reported for estimation of Ambroxol HCl alone and in combination with other drugs [20][21][22][23][24][25]. Likewise, in literature there are two of UVspectroscopic methods and one HPLC available for simultaneous analysis of ambroxol HCl and salbutamol sulphate in combined dosage form [26][27][28]. ...
Article
Full-text available
RP-HPLC method was developed for concurrent analysis of ambroxol HCl and salbutamol sulphate from tablet formulation. Analytes were separated with mobile phase consisting of mixture of methanol and water (0.1% triethylamine) in the ratio 50: 50 at a flow rate of 0.7 ml/min with Nucleosil (4.6 mm I.D x 250 mm) C18 column. The retention time of ambroxol HCl and salbutamol sulphate was found to be 3.61 and 6.20 min, respectively. The detection was carried out at 224 nm. The dynamic range for ambroxol HCl and salbutamol sulphate observed was 15-75 µg/ml and 1-5 µg/ml, respectively. The percent recovery obtained for ambroxol HCl and salbutamol sulphate were close to 100%. Obtained statistical data of results was found to satisfactorily.
... These methods include Uv-spectrophotometry, HPLC, UPLC, Gas chromatography, etc [8][9][10][11][12][13][14][15][16][17][18][19][20][21][22][23]. Literature survey revealed various analytical methods have been reported for estimation of salbutamol sulphate alone and in combination with other drugs [24][25][26][27][28][29]. Similarly, there are two of analytical methods reported for Ambroxol HCl alone and in combination with other drugs [30][31]. ...
Article
Full-text available
A simple UV-Vis Spectrophometric method was developed for the simultaneous determination of salbutamol sulphate and ambroxol HCl (AMB) from their combined dosage form. The method employs formation and solving of simultaneous equation using 242 nm and 272 nm as two analytical wavelengths (λMax of the drugs) of detection. Both the drugs obeyed Beer-Lambert’s law over the concentration range 1-50 μg/mL for salbutamol sulphate and 10-50 μg/mL for ambroxol HCl, respectively. The developed method was validated for Accuracy, Precision, Limit of Detection and Limit of Quantification as per ICH guidelines and results of analysis were validated statistically.
... The present research method precision was determined by three parameters such as inter-day, intra-day and method precision [15]. For determination of intra-day precision, the calibration curve of three different efinaconazole concentrations (50, 100 and 150 µg/mL) in triplicate were assessed within a single day period and subsequently % RSD for each concentration was calculated. ...
Article
The aim of current research work was to establish robust, sensitive, precise and selective reversed-phase high-performance liquid chromatography (RP-HPLC) method for the quantification of efinaconazole from microemulsion and microemulsion-gel based formulations for onychomycosis treatment. Chromatographic separation of efinaconazole was performed on Waters Inertsil® HPLC column, 5 µm (ODS-3V C18, 250 × 4.6 mm). The mobile phase was optimized as mixture of X and Y components in 20:80 v/v proportion (X component contains 0.01M phosphate buffer having pH 5.5 and acetonitrile in 75:25 v/v proportion and Y component contains acetonitrile) and the flow rate optimized at 1 mL min⁻¹. Efinaconazole detection and quantification was done at a wavelength of 210 nm using a ultra-violet (UV) detector. Linear relationship was observed in method calibration curve for the concentration range of 50–150 µg/mL with r² value >0.99. Different stress conditions experiments were carried out for the efinaconazole method development such as in acidic, basic, oxidation, photo, thermal, and humidity condition and no unknown degradation products interference were found during the estimation of efinaconazole. Further, the matrix effect of a microemulsion based excipients like diethylene glycol monoethyl ether, caprylcaproyl macrogol glycerides, and glyceryl caprylate has been overcame by present method of analysis with no excipient's interference. The method for analysis of efinaconazole was accurate, precise with average recovery rate of 98.6–101.6% and percentage RSD for all parameters of chromatographic system were found to be not more than 2.0%. Further, the method can be rapidly and effectively applied for the quantification of efinaconazole drug content from a microemulsion and microemulsion based gel formulations. Abbreviations: AUC, area under a curve; RP-HPLC, Reversed-phase high-performance liquid chromatography; ICH, International Council for Harmonisation; LOD, limit of detection; LOQ, limit of quantification; UV, ultra-violet; RSD, relative standard deviation; N, number of theoretical plates; Smix, surfactant mixture.
Article
This Review article is intended to highlight the analytical methods of Doxofylline in indivisual as well as combined pharmaceutical dosage form Doxofylline plays an important role in Asthma, COPD and various Respiratory diseases. Doxofylline is New generation long acting Oral methyl xanthine derivative. Doxofylline (7-(1.3 dioxolan-2ylmethy 1) 3.7 dihydro 13 dimethyl-1H purine 2. 6 Dione) is a newer generation xanthine with Broncho dilating and anti-inflammatory activities and for this reason it has been called Novofylline. Now these drugs are easily available in market in their indivisual form as well as combined Dosage form. Various analytical methods have been reported for the estimation of these drugs in their individuals as well as their combined Dosage form.
Article
Ambroxol hydrochloride (AMX) and guaifenesin (GFN) are approved drugs utilized to treat coughs through their potent mucolytic and expectorant properties. Due to their massive, combined administration in many illnesses, there is a persistent need for their concurrent estimation in different pharmaceutical formulations. Two sensitive, environmentally friendly spectrofluorimetric methods were developed. AMX was determined using the first method (I) without interference from GFN. This method depends on the quenching of Erythrosine B (EB) native fluorescence at 552 nm after excitation at 527 nm due to the formation of a non‐fluorescent AMX‐EB ion‐pair complex in Britton–Robinson buffer (BRB) solution pH (3.5). The concentration plot is linear over the 0.25–5.0 μg/mL range, with a mean percent found value of 99.74%. Method (II) depends on measuring the native fluorescence of aqueous GFN solution at two analytical wavelengths, either 300 or 600 nm, after excitation at 274 nm. Relative fluorescence intensity (RFI)–concentration plots are linear over the ranges of 0.02–0.5 and 0.1–2.0 μg/ml, with mean percent found at 99.96% and 99.91% at dual wavelengths, respectively. The proposed methods were successfully applied to assay both drugs in raw materials and different single and combined pharmaceutical formulations. These methods have been thoroughly validated following International Committee on Harmonisation (ICH) guidelines. National Environmental Methods Index, Analytical Eco‐Scale, and Green Analytical Procedure Index were used to prove greenness, thereby enhancing their applicability. The proposed techniques provide straightforward, precise, and cost‐effective solutions for routine formulation analysis in quality control laboratories.
Article
Full-text available
Objective: This study aims to develop a spectrophotometric method with the Ratio Difference method using ethanol pro analysis solvent to obtain the results of Dextromethorphan Hydrobromide (HBr) levels of Guaifenesin and Diphenhydramine Hydrochloride (HCl) in tablets. Methods: The Ratio Difference Sprctrophotography method involves dividing the mixture spectrum by the standard spectrum of each analyte and reducing the ratio to obtain a spectrum that does not depend on the concentration of the analyte used as a divider and can directly determine the levels of Dextromethorphan HBr, Guaifenesin, and Diphenhydramine HCl in the range 200-400 nm wavelength using experimentally calculated absorbance. Results: The maximum wavelengths of Dextromethorphan HBr, Guaifenesin, and Diphenhydramine HCl were obtained at 278 nm, 273 nm, and 252 nm, respectively. The average % accuracy obtained was 99.60% for Dextromethorphan HBr, 98.98% for Guaifenesin, and 100.32% for Diphenhydramine HCl in dosage forms. Conclusion: This method was successfully applied with simultaneous estimation to determine Dextromethorphan HBr, Guaifenesin, and Diphenhydramine HCl levels in tablet preparations and met the validation requirements.
Article
Background Worldwide, the prescriptions for asthma drugs are on the rise. However, anti-asthma drugs have side effects and can lead to fatal death at higher doses. Quite often, these drugs are abused as growth promoters in poultry/livestock as well as by athletes to enhance their performance. Consequently, it is vital to design uncomplicated, portable, rapid and highly sensitive means of detecting these anti-asthma drugs in pharmaceutical formulations and other sample matrices. This review highlights the use of electrochemical sensors as alternative methods to conventional analytical techniques for detecting anti-asthma drugs in pharmaceuticals and biological fluids. Methods Literature covering diverse detection methods for anti-asthma drugs were reviewed to provide background information in this area of research. Next, the literature survey focused primarily on the emergence of the nanotechnology platform, including the strengths and weaknesses of this approach. Finally, a perspective on the future direction of this method was summarized. Results Electrochemical sensors offer several advantages over conventional methods, which require long and tedious extraction, pre-concentration and clean up steps. Moreover, electrochemical sensor techniques are less expensive, easy to operate and avoid the need for harmful reagents known to generate a huge amount of non-environmental friendly chemicals. Conclusion Nanotechnology-based electrochemical sensors represent a promising platform for analysing anti-asthma drugs in pharmaceuticals and biological fluids given their beneficial effects such as low cost, use of less health hazardous materials, and compatibility with environmental health.
Article
Full-text available
A RP-HPLC method has been developed for the estimation of glipizide (GLP). The proposed method is based on the separation of the drug in reversed-phase mode using BDS HYPERSIL C18 (4.6 mmø×250 mm) analytical column, mobile phase methanol:water 70:30 V/V, at the flow rate of 1.0 mL min-1 and detection wavelength 222 nm. GLP was well resolved and retained at t = 3.86 minutes. This RP-HPLC method was validated as per the recommendations of ICH Revised Q2(R1) guidelines of analytical method validation, in order to prove that the new analytical method meets the reliability characteristics. The method characteristics showed the capacity of an analytical method to keep, all over the time, the basic standards for validation: selectivity, linearity, precision, accuracy and sensitivity. The method was found linear over the range 1-7 µg mL-1. The LOD and LOQ were 0.5281 and 1.761 µg mL-1 for GLP. The validated method was successfully used for quantitative estimation(assay) of GLP from in-house formulation and marketed formulations.
Article
Ambroxol (AMB) is a member of the expectorant class, widely used as a secreolytic agent in patients to break up secretions. AMB is rapidly and effectively distributed from blood to tissue. The lungs have the highest concentration of AMB; accumulation of AMB in human lung tissue was detected at concentrations 15- to 20-fold greater than those reported in the circulation. Because of its wide range of actions and therapeutic applications may be worth looking into, particularly for respiratory symptoms, antioxidant, anti-inflammatory, influenza, and rhinovirus infections. Though several analytical methodologies have been established and confirmed for the AMB analysis in matrices of pharmaceutical and biological origins, novel sustainable, and economical methods are still to be choice of protocol to increase its sensitivity, reliability, and repeatability. Therefore, the present review offers an overview of critical analytical aspects regarding the HPLC, LC-MS/MS, HPTLC, capillary electrophoresis, spectrophotometry, and electrochemical methods for quantifying AMB in pharmaceutical and biological samples. Furthermore, this review will thoroughly discuss the physicochemical properties, stability, extraction conditions, instrumentation, and operational parameters of the targeted analyte. As a result, for the first time, this review complies with vital background information and an up-to-date interpretation of research undertaken by anticipated methodologies examined and implemented for the pharmaceutical analysis AMB.
Article
A simple, step by step, cost-effective, accurate, sensitive, and selective validated High Performance Thin Layer Chromatographic method for simultaneous determination of Terbutaline sulphate, Ambroxol hydrochloride, and Guaifenesin in syrup formulation has been developed and validated. HPTLC separation was achieved on Merck aluminum HPTLC plates precoated with silica gel 60 F254. The solvent system comprised of Chloroform: Methanol: Ethyl acetate: Acetic acid: Formic acid (7.0:1.4: 0.8:1.0:0.5 v/v). Densitometric detection wavelength at 200 nm was used in reflectance-absorbance mode. The retention factors were found to be 0.32±0.02, 0.55± 0.02, and 0.72±0.02, for Terbutaline sulphate, Ambroxol hydrochloride, and Guaifenesin respectively. Results were found to be linear over a range of 200 - 700ng band-1, 1000 - 7000ng band-1, and 400-1200ng band-1 for Terbutaline sulphate, Ambroxol hydrochloride, and Guaifenesin, respectively. The percent assay was found to be 98.47%, 98.47%, and 99.23%, for Terbutaline sulphate, Ambroxol hydrochloride, and Guaifenesin, respectively in marketed formulation. The developed densitometric method was validated by following the International Council on Harmonisation (ICH) guideline. The developed and validated chromatographic method can be applied for routine quality control of Terbutaline sulphate, Ambroxol hydrochloride, and Guaifenesin in the combined syrup dosage form used in study.
Article
Full-text available
A simple and sensitive RP-HPLC method developed for estimation of Polmacoxib in bulk by using a high performance liquid chromatography with PDA detector using Phenomenex luna C18 column (250mmx4.6mm), 5 µm; mobile phase comprises of Water : ACN as (1:1) at the flow rate 1.0 ml/min and the wavelength of detection 238 nm and eluted at 8.12 minutes. The proposed method is validated for specificity, Linearity, Precision, accuracy, ruggedness, and Robustness. All the parameters were found within the acceptable limits. RP-HPLC method was a simple, reliable economic and acceptable and it confirmed that method is suitable for the intended use for routine quality control and assay of drugs. This method is successfully applied for the determination of commercial dosage form capsule preparation. This method is validated as per ICH (International conference on harmonization) Guidelines. Keywords: Polmacoxib, RP-HPLC, ICH, PDA Detector, Precision
Article
In this review article, we will introduce all reported methods that have been developed for determination of certain anti-tussive and anti-histaminic drugs such as salbutamol, ambroxol and fexofenadine in their pure form, combined form with other drugs, combined form with degradation products, and in biological samples. We also will shed the light on the most important combination of drugs that are used for treatment of asthma and related diseases.
Article
In this study, simultaneous determination of acetaminophen (ACT), phenylephrine (PHE), and guaifenesin (GUA) in synthetic mixtures and syrup formulation was performed using spectrophotometry technique along with continuous wavelet transform (CWT) and derivative transform (DT). Among various wavelet families, Daubechies (Db2), Symlet (Sym4), and Coiflet (Coif2), were selected to analyze ACT, PHE, and GUA, respectively. Mean recovery and root mean square error (RMSE) of CWT method were found 100.19%, 98.96%, 95.35% and 0.00023, 0.0026, 0.0031 for ACT, PHE, and GUA, respectively. For DT method, the first derivative absorption spectra were chosen for determining ACT, PHE, and GUA at 237, 224, and 219 nm, respectively. Mean recovery values were achieved between 97.15% and 100.35%. Also, limit of detection (LOD) and limit of quantification (LOQ) were obtained between 0.0138-0.1507, 0.0012-0.0123 μg ml⁻¹ and 0.0695-0.7786, 0.0025-0.0767 μg ml⁻¹ for CWT and DT methods, respectively. These proposed procedures were compared with the high-performance liquid chromatography (HPLC) as a reference technique via analysis of variance (ANOVA). The results did not show a significant difference between the methods. The suggested methods are simple and cost-effective for the quantitative assessment of three-component mixture.
Article
Full-text available
Guaifenesin is an expectorant and it is use to treat cough and congestion caused by the common cold, bronchitis, and breathing illness. The drug is official in Indian Pharmacopoiea, British Pharmacopoeia, and United States Pharmacopoeias. This article reviews the different analytical methods available for detection of Guaifenesin alone and in combination from various pharmaceutical formulations. They are many analytical techniques have been reported for simultaneous estimation of Guaifenesin and its combined pharmaceutical dosage form but only fewer methods have been reported for estimation of Guaifenesin alone. Some of those techniques are UV spectrophotometry, high-performance liquid chromatography (HPLC), high-performance thin layer chromatography (HPTLC), liquid chromatography-mass spectrometry (LC-MS), gas chromatography (GC), and ultraperformance liquid chromatography (UPLC). Amongst, various analytical methods are available for the quantification of single and multicomponent dosage forms.
Article
Full-text available
A simple, rapid, isocratic, and versatile liquid chromatographic method was developed for the simultaneous determination of bromhexine, guaifenesin, ambroxol, salbutamol/terbutaline, pseudoephedrine, triprolidine, and chlorpheniramine maleate in cough–cold syrups commonly marketed in Kenya. Separation was achieved using a Gemini® NX C18 column (250 × 4.6 mm, 5 μm) maintained at 40 °C and a mobile phase consisting of acetonitrile-0.25 M sodium hexanesulphonate-0.2 M ammonium acetate, and pH 3.0-water (35:4:10:51, % v/v/v/v) delivered at 1.0 mL min⁻¹. The eluents were monitored by means of UV detection at 254 nm. During validation, the method satisfied the International Committee on Harmonization acceptance criteria for linearity, sensitivity, precision, accuracy, and robustness. The developed liquid chromatographic method was applied in the analysis of nine commercial samples obtained from Nairobi City County, Kenya. Extraction procedures were not applied during the assay of the samples, thus significantly shortening the analysis time.
Article
Full-text available
Pharmaceutical Cough Cold Preparations like syrup are widely used worldwide and mostly in countries like India. Aim and Objective of the study is to develop simple, precise, accurate, rapid and sensitive Method of Reverse Phase High Performance Liquid Chromatography (RP-HPLC) and High Performance Thin Layer Chromatography (HPTLC) for simultaneous estimation of Ambroxol HCl (AMB), Dextromethorphan HBr (DEX) and Guaifenesin (GUA) in Pharmaceutical Cough Cold Preparation and statistical comparison of both method was done. For RP-HPLC method Hibar RP-C18 (250mm × 4.6mm i.d. with particle size of 5μm) analytical column was used. The mobile phase composition used for RP-HPLC method was Acetonitrile - Methanol - 10mM Phosphate Buffer - 0.3% Triethyl Amine (25:15:60 v/v) and pH was adjusted to 3 using Orthophosphoric Acid. Flowrate was kept 1 mL/min. Detection was done at 205 nm using PDA detector. Linearity range for RP-HPLC method was found to be 3-10.5 μg/ml, 2-7 μg/ml and 10-35 μg/ml for AMB, DEX and GUA respectively. In HPTLC method Merck HPTLC plates precoated with 60F254 silica gel on aluminium plates were used as stationary phase. Mobile phase used in HPTLC method was Toluene - Methanol - Chloroform - Glacial Acetic Acid (6.5:1.5:1.5:0.5 v/v/v/v). Detection was done using Camag TLC scanner at 275 nm. Linearity range was found to be 1.5-3 μg/band, 1-2 μg/band and 5-10 μg/band for AMB, DEX and GUA respectively for HPTLC method. Statistical comparison of RP-HPLC and HPTLC was done by application of t-Test to recovery data of both methods. Finally concluded that A novel RP-HPLC and HPTLC methods were developed for simultaneous estimation of AMB, DEX and GUA in syrup dosage form. Both the method gives the good resolution for all three drugs. The developed method was validated and found to be sensitive, accurate, specific and reliable for simultaneous estimation of AMB, DEX and GUA in syrup dosage form. The proposed method can be used effectively in routine analysis.
Article
Full-text available
A new liquid chromatographic method has been developed and validated for the determination of terbutaline sulfate (TLS), guaifenesin (GEN) and ambroxol HCl (AML), for its potential impurities in drug substances and drug products. Efficient chromatographic separation was achieved on X-Terra RP-18 column with a simple mobile phase combination containing a gradient mixture of solvents A and B at a flow rate of 1.0 mL min(-1) and quantitation was carried out using ultraviolet detection at 222 nm with column temperature of 35 degrees C. The resolution between TLS, GFN and AML, its associated impurities was found to be greater than 1.5. Regression analysis shows an r value (correlation coefficient) greater than 0.998. This method was capable to detect all the process impurities of TLS, GFN and AML, at a level below 0.015% with respect to a test concentration of 0.125, 5.0 and 1.5 mg mL(-1), respectively. The % RSD for the inter-day and intra-day precisions for all the impurities of TLS, GFN and AML were found to be less than 3.0. The method has shown good, consistent recoveries. The drugs were subjected to stress conditions of acid, base, water hydrolysis, oxidation, photolysis and thermal degradation, as prescribed by international conference on harmonization (ICH). (C) 2012 Production and hosting by Elsevier B.V. on behalf of King Saud University.
Article
Full-text available
A simple and precise liquid chromatography method for the simultaneous estimation of Salbutamol sulfate, Guaifenesin, and Ambroxol hydrochloride in combined tablet dosage form was developed and validated. The chromatographic separation of the drugs was achieved with a Princeton sphere C-8 25 cm × 4.6 mm (Rankem) analytical column using buffer and methanol (58:42 v/v) as the mobile phase. The buffer used in mobile phase contained 0.1 M potassium dihydrogen phosphate and its pH was adjusted to 4.5 with 10% ortho-phosphoric acid. The instrument was set at a flow rate of 1.0 mL min, column at ambient temperature, and the wavelength of UV-visible detector at 220 nm. The method showed excellent linearity over a range of 5–35 µg mL for all the drugs. The correlation coefficients for Salbutamol sulfate, Guaifenesin, and Ambroxol hydrochloride were noted to be 0.9998, 0.9998, and 0.9995, respectively, and the mean recovery values were found to be 99.53%, 100.28%, and 100.05%, respectively. The proposed method could be suitable for quantitative determination of these drugs in pharmaceutical preparations and also for quality control in bulk manufacturing. The intermediate precision data was subjected to statistical analysis (F-test and t-test at 95% confidence level).
Article
Full-text available
This paper presents different HPLC methods for the simultaneous determination of some guaiphenesin-containing cough-cold preparations. Three pharmaceutically available combinations were analyzed: salbutamol sulfate (SAL) and guaiphenesin (GUA), combination I; ascorbic acid (ASC), paracetamol (PAR) and guaiphenesin (GUA), combination II; and theophylline anhydrous (THE), guaiphenesin (GUA) and ambroxol hydrochloride (AMB), combination III. A 250×4.6mm C-18 column was used for all combinations. The mobile phase for the three combinations consisted of a mixture of methanol and 0.01M aqueous phosphate buffer solution. The pH of the mobile phase was adjusted to 3.2, 6.2 and 3.8 for combinations I, II and III, respectively. The proposed HPLC methods were successfully applied to the determination of the investigated drugs, both in synthetic mixtures and in pharmaceutical preparations, without any matrix interference and with high precision and accuracy. Different aspects of analytical validation are presented in the text.
Article
An ior-pair HPLC method has been developed and validated for simultaneous determination of pseudoephedrine HCl (PSEU), guaifenesin (GUA) and dexchlorpheniramine maleat (DEX) in cough and cold syrup. This method is based on the interaction of analits and ion-pairing agent and was achieved on the Phenomenex C18 column (250 x 4.6 mm, 5 μm) using an isocratic mobile phase consisting of methanol:acetonitrile: 10mM Na-pentansulphonate at pH 4,0±0,1 (55:5:40 v/v/v). The analysis was performed at a flow rate of 1 mL/min, using UV detection at 218 nm. The result showed good linearity over the range of 96 – 144 μg/mL for PSEU, 320 – 480 μg/mL for GUA and 6.4 – 9.6 μg/mL for DEX with correlation coefficients more than 0.999. The mean value of recovery were 100.415% for PSEU, 99.898% for GUA and 100.822 for DEX. The validated method was successfully applied to determine these compounds in two commercial cough and cold syrup without being interrupted by the presence of other excipients. Small variations in method condition did not provide a significant difference to the concentration indicated that the method is robust. © 2016, International Journal of Pharmaceutical and Clinical Research. All rights reserved.
Article
The present paper describes a simple, accurate and precise reversed phase HPLC method for rapid and simultaneous quantification of Terbutaline Sulphate, Bromhexine Hcl and Guaifenesin in a cough syrup formulation. Separations were carried out on a phenomenex Luna C18 column (250 X 4.6 mm ID), 5 μm particle size. A isocratic elution system was developed using acetonitrile-methoanol-buffer (350:450:250 v/v). The elution of the analytes was achieved in less than 15 min with a flow rate of 1.2 ml/min. Detection was by UV absorbance at a wavelength of 220 nm. Quantification of the components in actual syrup formulations was calculated against the responses of freshly prepared external standard solutions. Different analytical performance parameters such as linearity, precision, accuracy, limit of detection, limit of quantification, and robustness were determined according to international conference on harmonization ICH Q2B guidelines. All the parameters of validation were found in the acceptance range of ICH guideline.
Article
This study proposes a method for simultaneous estimation of Ambroxol HCl, Guaifenesin and Terbutaline sulphate in syrup form. The study was done by combining three spectrophotometric methods viz use of specific absorbance [A 1%, 1cm], second order derivative and colorimetry. Absorption of Guaifenesin and Terbutaline sulphate were found to be zero at 307.5nm, thus enabling the measurement of Ambroxol HCl, using specific absorbance in zero order spectrum. Applying the second order derivative, the amplitude of Guaifenesin was measured at 279.4nm, while Ambroxol HCl and Terbutaline sulphate were at zero cross point. For colorimetric measurement of Terbutaline Sulphate, a colored substance was obtained by coupling the oxidized product of Terbutaline sulphate with 4-aminoantipyrine and its absorption was measured at 550nm. The proposed method was statistically validated in accordance with ICH guidelines and results were found to be satisfactory for accuracy, precision and specificity.
Article
The performance of three phenylcarbamate based chiral stationary phases was evaluated for the optimum separation of guaifenesin enantiomers. Resolution, enantioselectivity and capacity factors were compared simultaneously using four factor three level experimental design. Chiralcel OD provided the highest resolution and selectivity but the lowest capacity factor for the less retained enantiomer along with peak broadening for the more retained enantiomer. On the other hand, Lux amylose-2 provided the lowest parameters. Optimum resolution and selectivity with the highest capacity factors was provided by Lux cellulose-2 as stationary phase and ethanol/hexane (15:85 v/v) as a mobile phase at a flow rate of 1.2 mL min-1 and column temperature at 19 °C. Extended separation of guaifenesin enantiomers and ambroxol HCl was accomplished using the same optimized chromatographic conditions. The proposed methods were applied for the determination of analytes in syrup formulation with high specificity. The method was validated as per International Conference on Harmonization guidelines and compared with a reported HPLC method.
Article
The effects of terbutaline sulphate were studied in 30 patients who presented with chronic cough at an allergy clinic. After a three week baseline period terbutaline and its placebo were given for two periods of three weeks each in a randomised, double blind, crossover manner. Patients kept a daily record of day and night cough scores and peak expiratory flow readings. Twenty one patients responded to terbutaline; placebo produced no significant effect. Both day and night cough scores (p less than 0.001) and peak expiratory flow rates were significantly improved (p less than 0.05) by the end of the first week of treatment with terbutaline. This improvement was achieved with only a fairly small change in airway calibre.
Clinical Reasoning in Primary Care. Pharmacotherapeutics W.B. Saunders Co
  • K Gutierrez
Gutierrez K. Clinical Reasoning in Primary Care. Pharmacotherapeutics W.B. Saunders Co; 2007.
Stability indicating RP-HPLC method for the determination of terbutaline sulphate, guaifensin, ambroxol hydrochloride and preservatives content in liquid formulations
  • H R Bapatu
  • M R Kumar
  • U R Mallu
  • Hkr Ganthi
  • Cmr Kota
  • V R Pyreddy
Bapatu HR, Kumar MR, Mallu UR, Ganthi HKR, Kota CMR, Pyreddy VR. Stability indicating RP-HPLC method for the determination of terbutaline sulphate, guaifensin, ambroxol hydrochloride and preservatives content in liquid formulations. J Pharm Res 2011;4(11):4117-22.
Development and validation of reverse phase HPLC method for simultaneous estimation of ambroxol HCl, guaifenesin and levosalbutamol in syrup
  • C P Nirav
  • B P Dipti
  • K C Pruthviraj
Nirav CP, Dipti BP, Pruthviraj KC. Development and validation of reverse phase HPLC method for simultaneous estimation of ambroxol HCl, guaifenesin and levosalbutamol in syrup. Pharm Anal Qual Assur 2013;2:1-6.
High performance liquid chromatography method for simultaneous determination of terbutaline sulphate, guaifenesin, and ambroxol hydrochloride in formulations
  • Kpl Shenoy
  • K S Krishnamurthi
  • I Vasundhara
Shenoy KPL, Krishnamurthi KS, Vasundhara I. High performance liquid chromatography method for simultaneous determination of terbutaline sulphate, guaifenesin, and ambroxol hydrochloride in formulations. Indian Drugs 2001;38(8):428-32.
International Council of Harmonization, Q2B validation of analytical procedures: methodology and availability
International Council of Harmonization, Q2B validation of analytical procedures: methodology and availability. Fed Regist 1997;62(96):27463-7.