Micellar Liquid Chromatographic Method Research Articles

A Mixed Micellar Liquid Chromatography with Direct Injection for Rapid Analysis of Eight Sulfonamides in Milk

In this work, an isocratic mixed micellar liquid chromatography method was first applied to the separation of eight sulfonamides in milk. Mixed anionic and nonionic surfactants were used as mobile phase additives. Because proteins in the milk can be dissolved by the micelles, the milk samples can be directly injected into the chromatographic system after being simply diluted 10 times with 0.1 M sodium dodecyl sulfate solution. Besides, three-phase equilibrium theory was firstly used to explain the retention mechanism of sulfonamides in the mixed micellar liquid chromatography. The optimized mobile phase was an aqueous solution (0.04 M sodium dodecyl sulfate and 0.01 M polyoxyethylene lauryl ether) containing 20 mM NaH2PO4 with 10% (v/v) of n-propanol at pH 3.0. The separation was performed on a Venusil XBP C18 column (250 × 4.6 mm, i.d., 5 μm). The proposed mixed micellar liquid chromatography method was validated in terms of linear ranges (20–2500 μg/L), limit of detections (1.9–8.0 μg/L), limit of quantitations (6.1–27 μg/L), recoveries (84–105%), intra- and inter-precisions (RSD < 6.0%, RSD < 9.3%). The established method, which is rapid, low-cost, and environmentally friendly, provides an alternative way for rapid separation of sulfonamides within 15 min, and it does not require the complex gradient elution.

Micellar high performance liquid chromatographic method for separation and validation of two anti-hepatitis C- virus drugs in pure form, human plasma and human urine

In the present study, an eco- friendly micellar liquid chromatographic technique was validated for separation and quantification of two drugs; namely ribavirin (RIV), and sofosbuvir (SBV) in pure form, pharmaceuticals containing them, human plasma and human urine. These drugs are administered co-administered for treatment of Hepatitis C virus (HCV) that causes hepatitis C in humans. These drugs were separated using Nucleosil 100-5 phenyl column. Sodium dodecyl sulphate (SDS) solution (0.05M, pH 7.0) containing triethylamine (0.3%) and n-butanol (10%) was used as a mobile phase with 1.2 mLmin-1 flow rate and 215nm detection wavelength. Nine minutes were required for resolving the two drugs from the matrix. The method showed good linearity for RIV and SBV with correlation coefficients (r2) more than 0.9996 within the concentration ranges of (20-400) and (40-400) ngmL-1 in pure form, (30-300) and (50-300) ngmL-1 in human plasma and (20-400) and (40-400) ngmL-1 in human urine, respectively. The recommended method was applied for examination of RIV and SBV in pure and pharmaceuticals. The obtained results were statistically matched with reported methods with no significant differences. Also, the recommended method was effectively applied for estimation of both drugs in spiked human urine and plasma without purification or extraction steps and real samples of plasma and urine of humans having therapy of RIV and SBV, as well as, performing tablets dissolution-rate tests with satisfactory results.

Mixed micellar liquid chromatographic method for simultaneous determination of norfloxacin and tinidazole in pharmaceutical tablets

A new green mixed micellar liquid chromatographic method was developed, validated, and successfully applied for the determination of norfloxacin and tinidazole in bulk and in pharmaceutical dosage form. The developed method used the anionic surfactant; sodium dodecyl sulphate and the neutral surfactant polyoxyethylene (23) lauryl ether without need of organic solvent in the mobile phase. Optimization of the chromatographic condition was performed by 23 full factorial design. Chromatographic separation and quantitation was performed on ODS Hypersil® column (250 × 4.6 mm, 5 μm). Mixed-micellar mobile phase consisted of 0.14 M SDS, 0.03 M Brij-35 and 0.3% triethylamine. pH of the mobile phase was adjusted to 2.9 by orthophosphoric acid. The flow rate was 1 mL/min. The injection volume was 20 μL. UV detection was performed at 313 nm. Linearity ranges were found to be 2–10 μg/mL and 2–12 μg/mL for norfloxacin and tinidazole, respectively. The developed method was validated and successfully applied to the simultaneous determination of both drugs in their tablet. The mean percentage recovery ± S.D. values were found to be 97.745 ± 0.664 and 100.441 ± 1.379 for norfloxacin and tinidazole, respectively. The assay results obtained were statistically compared to those obtained by a reported method and good agreement was observed. The present method offers significant advantages compared to previously reported chromatographic methods concerning column efficiency, selectivity and resolution. The green property of the method was evaluated. The method is verified to obtain excellent greenness. The calculated analytical Eco-Scale of the method was also compared to those of other reported liquid chromatographic methods.

Assessment of the greenness of spectrophotometric and micellar liquid chromatographic methods using two approaches: Application to pharmaceutical analysis of hydrochlorothiazide and telmisartan

Recently the focus of analytical community is to eliminate or reduce the usage of hazardous chemicals; consequently, two ecofriendly, rapid, selective and cost-effective methods are developed for the simultaneous determination of hydrochlorothiazide (HCZ) and telmisartan (TEL). The first method is based on micellar high pressure liquid chromatography using an ecofriendly micellar mobile phase consists of 0.06 M sodium dodecyl sulfate (SDS), 12% v/v n-propanol and 0.3% v/v triethylamine (TEA) at pH 6.0 pumped at a flow rate of 2 mL/min. Rivaroxaban (RIV) is used as an internal standard (I.S). The method gives linear correlation over concentration ranges of 0.8–20.0 μg/mL and 1.0–20.0 μg/mL for HCZ and TEL, respectively. The mean percentage recovery for HCZ is 100.60 ± 0.92 while for TEL is 100.07 ± 1.16. The second method is based on absorbance ratio (Q-absorbance) technique which depends on measuring the absorbance at two certain wavelengths, one of which is the isoabsorptive point and the other is the λmax of one of the two drugs. Methanolic solutions of HCZ and TEL show their isoabsorptive points at 264.6 nm and 277.3 nm while the λmax of HCZ in methanol is 270 nm. The two drugs obey Beer-Lambert law over the concentration ranges of 1.0–20.0 μg/mL for HCZ and TEL, respectively. For HCZ, the mean percentage recovery is 99.86 ± 0.87 while for TEL it is 99.83 ± 0.94. The spectrophotometric method does not need the addition of any chemical reagents and is carried out without heating or extraction steps. Both methods are successfully applied to the analysis of both drugs in their combined tablets. The results are validated according to official guidelines. Statistical evaluation of the results achieved by the developed and comparison official methods confirms the high accuracy and precision of the developed methods as indicated by student t-test and variance ratio F-test, respectively. Moreover, the greenness of the developed methods is assessed using suitable analytical Eco-Scale and greenness profile, and comparison with the previously published methods has been carried out to indicate priority of the proposed procedures.

Green micellar HPLC-fluorescence method for simultaneous determination of metoprolol and amlodipine in their combined dosage form: Application on metoprolol in spiked human plasma

A fast, sensitive and reliable green micellar liquid chromatographic method has been developed and validated for simultaneous determination of metoprolol (MET) and amlodipine (AMD). Separation was performed on X-Bridge ODS column (150 × 4.6 mm, 5 μm particle size) using a micellar mobile phase consisting of 100 mM sodium dodecyl sulfate, 20 mM sodium dihydrogen phosphate buffer pH 3.0 and 10% v/v n-butanol. The fluorescence detector was set at 275/ 303 nm (excitation/ emission) for MET and 364/ 455 nm (excitation/emission) for AMD. A linear response was obtained over the ranges of 0.1–10 μg/mL and 0.2–2 μg/mL for MET and AMD, respectively. The method reached limits of detection of 20 ng/mL for MET and 50 ng/mL for AMD. The proposed method was successfully employed for the determination of the two drugs in their combined pharmaceutical dosage form and in addition, it was extended for the determination of MET in spiked human plasma. Furthermore, the green character of the developed method was evaluated using the new tool “green analytical procedure index (GAPI)”. The developed method was verified to be an excellent green method.

Optimization and Validation of a Chromatographic Method for the Quantification of Isoniazid in Urine of Tuberculosis Patients According to the European Medicines Agency Guideline.

Isoniazid is a drug that is widely used against tuberculosis. However, it shows high interpatient variability in metabolism kinetics and clinical effect, which complicates the prescription of the medication and jeopardizes the success of the therapy. Therefore, in a specific patient, the pharmacokinetics of the drug must be elucidated to decide the proper dosage and intake frequency to make the drug suitable for therapeutic drug monitoring. This can be performed by the quantification of the drug in urine as this process is non-invasive and allows the effects of long-time exposure to be inferred. The paper describes the development of a micellar liquid chromatographic method to quantify isoniazid in urine samples. Extraction steps were avoided, making the procedure easy to handle and reducing the waste of toxic organic solvents. Isoniazid was eluted in less than 5 min without interference from other compounds of the urine using a mobile phase containing 0.15 SDS–12.5% 1-propanol (v/v)–Na2HPO4 0.01 M buffered at pH 7, running at 1 mL/min under isocratic mode through a C18 column with the detection wavelength at 265 nm. The method was validated by following the requirements of the Guidelines on Bioanalytical Method Validation issued by the European Medicines Agency (EMA) in terms of selectivity, calibration curve (r2 = 0.9998 in the calibration range (0.03–10.0 μg/mL), limit of detection and quantification (10 and 30 ng/mL respectively), precision (<16.0%), accuracy (−0.9 to +8.5%), carry-over, matrix effect, and robustness. The developed method was applied to quantify isoniazid in urine samples of patients of an Indian hospital with good results. The method was found to be useful for routine analysis to check the amount of isoniazid in these patients and could be used in its therapeutic monitoring.

Micellar liquid chromatographic method for the simultaneous determination of citalopram hydrobromide with its two demethylated metabolites. Utility as a diagnostic tool in forensic toxicology

A micellar liquid chromatographic method has been developed for the simultaneous determination of citalopram hydrobromide (CTA) with its two demethylated metabolites namely; desmethyl citalopram hydrochloride (DCTA) and didesmethyl citalopram tartrate (DDCTA). Separation was conducted on a C18 column using a mobile phase composed of 0.18 M sodium dodecyl sulphate (SDS), 15% 1-propanol, 0.3% tri-ethylamine, adjusted to pH 4 with 0.2 M o-phosphoric acid and adopting UV detection at 240 nm. Analysis was performed at 60 °C applying a flow rate of 2 mL/min. The proposed method was linear over the concentration ranges of 1.0–200.0, 0.6–200.0, and 0.5–200.0 μg/mL for CTA, DCTA, and DDCTA respectively, with corresponding limits of detection (LOD) of 0.5, 0.4, and 0.3 μg/mL and limits of quantification (LOQ) of 0.8, 0.5, and 0.4 μg/mL. The method was fully validated which allowed its application for the determination of CTA in its tablets. Moreover, the proposed method was extended to assay CTA with its metabolites in rat tissue organs samples which allowed the method to be used as a diagnostic tool in forensic toxicology.

Investigation of anti-Hepatitis C virus, sofosbuvir and daclatasvir, in pure form, human plasma and human urine using micellar monolithic HPLC-UV method and application to pharmacokinetic study

Simultaneous determination of sofosbuvir (SOF), and daclatasvir (DAC) in their dosage forms, human urine and human plasma using simple and rapid micellar high performance liquid chromatographic method coupled with UV detection (HPLC-UV) had been developed and validated. These drugs are described as co-administered for treatment of Hepatitis C virus (HCV). HCV is the cause of Hepatitis C and some cancers such as liver cancer (hepatocellular carcinoma) and lymphomas in humans. Separation and quantitation were carried out on anonyx™ C8 monolithic (100 × 4.6 mm (i.d.) analytical column maintained at 25 °C. The mobile phase consisted of 0.1 M sodium dodecyl sulfate (SDS) solution containing 20% (V/V) n-propanolol and 0.3% (V/V) triethylamine and pH was adjusted to 6.5 using 0.02 M phosphoric acid, respectively. The retention times of SOF and DAC were 4.8 min, and 6.5 min, respectively. Measurements were made at flow rate of 0.5 mL/min with injection volume of 20 μL and ultraviolet (UV) detection at 226 nm. Linearity of SOF and DAC was obtained over concentration ranges of 50–400, and 40–400 ng/mL, respectively in pure form, 60–300 and 50–300 ng/mL, respectively for human plasma and over 50–400, and 40–400 ng/mL, respectively for human urine with correlation coefficient >0.999. The proposed method demonstrated excellent intra- and inter-day precision and accuracy. The suggested method was applied for determination of the drugs in pure, dosage form, and in real human plasma, real human urine and drug-dissolution test of their tablets. The obtained results have been statistically compared to reported method to give a conclusion that there is no significant differences.

Micellar HPLC method for the simultaneous determination of three anticonvulsant drugs in dosage forms and biological fluids. Application to dissolution-rate testing

This work describes a micellar liquid chromatographic method which was developed and validated to determine simultaneously three structurally-related antiepileptic drugs; namely carbamazepine (CMZ), oxcarbazepine (OCZ) and eslicarbazepine acetate (ECZ). The analysis was achieved using a phenyl column (250mm×4.6mm i.d., 5μm particle size), a mobile phase consisting of a mixture of 0.3% triethylamine and 10% n-butanol in a solution of 0.05M sodium dodecyl sulphate adjusted to pH 7.0 using 0.02M orthophosphoric acid. The mobile phase was pumped at a flow rate of 1.5mLmin-1 and detection was adjusted at 215nm. The method showed good linearity (r2>0.998) over the concentration ranges of 0.1-10 for CMZ and OCZ and 0.2-20μgmL-1 for ECZ. The suggested method was successfully applied for the analysis of the studied drugs in their dosage forms and for the determination of CMZ and OCZ in spiked human urine and plasma without prior extraction. The proposed method was further extended to the analysis of real samples of plasma and urine of volunteers receiving therapy of CMZ and OCZ. Furthermore, the method was successfully applied to tablets dissolution-rate testing, and the results were satisfactory.

Simultaneous Determination of Gatifloxacin and Prednisolone in their Bulk Powder, Synthetic Mixture and Their Combined Ophthalmic Preparation Using Micellar Liquid Chromatography

A simple rapid and accurate micellar high performance liquid chromatographic method was improved and validated for the analysis of mixture containing gatifloxacin sesquihydrate (GTF) and prednisolone acetate (PRED) in their synthetic mixture and their combined preparation. The separation was achieved using a C18 column, micellar mobile phase consisted of 0.2 M sodium dodecyl sulfate, 12.5% n-propanol and 0.3% triethylamine in 0.02 M orthophosphoric acid at pH 7.0 at a flow rate of 1 ml/min with UV detection at 270 nm. The proposed method was found to be rectilinear over the concentration ranges of 5.0-45 μg ml-1 and 10-50 μg ml-1 with recovery percentage of 99.95 ± 0.82 and 100.07 ± 0.84 for GTF and PRED, respectively. The separation of both drugs was accomplished in a very short chromatographic run (<5 min), the method is reproducible (R.S.D. < 1.0%) and show satisfactory resolution between GTF and PRED (Rs) = 1.67. The developed method was validated according to International Conference on Harmonization (ICH) guidelines. The limit of detection of the proposed method was 0.33 and 0.21 μg ml-1, and the limit of quantitation was 0.99 and 0.64 μg ml-1 for GTF and PRED, respectively.

A STABILITY INDICATING MICELLAR LIQUID CHROMATOGRAPHIC METHOD FOR THE DETERMINATION OF DEFERASIROX IN SOLUBILIZED SYSTEM

A simple, isocratic and stability indicating micellar liquid chromatographic (MLC) method containing a surfactant solution above its critical micellar concentration (CMC) was developed and validated for determination of Deferasirox (BTBA) content in active pharmaceutical ingredient and its pharmaceutical formulations. The analysis was performed in on isocratic mode at 400C temperature through Thermo Hypersil ODS 100mmA—4.6mm, 3 µm particle size columns. The UV detection wavelength was set at 250 nm in the mobile phase containing 0.1 M Cetyl trimethyl ammonium bromide (CTAB) buffer (pH – 2.5) and 10% 1-butanol. The method was successfully validated following as per the requirements of ICH guidelines. The proposed method was successfully applied as stability indicating method for determination of BTBA under different stressed conditions. The method allows accurate and reliable determination of BTBA for drug stability assay in pharmaceutical investigations.

Simultaneous Determination of Tizanidine, Nimesulide, Aceclofenac and Paracetamol in Tablets and Biological Fluids Using Micellar Liquid Chromatography.

A simple, sensitive and rapid micellar liquid chromatographic method was developed and validated for simultaneous determination of four drugs, namely, paracetamol (PAR), tizanidine (TZD), aceclofenac (ACF) and nimesulide (NMD). Good chromatographic separation was achieved using Cyano column and micellar mobile phase consisting of 120 mM sodium dodecyl sulfate, 25 mM phosphate buffer and 10% (V/V) butanol. The pH was adjusted to three using phosphoric acid. The total retention time was below 10 min. The analysis was performed at a flow rate of 1 mL/min and a column temperature of 40°C with direct UV detection at 230 nm. Diclofenac sodium was used as the internal standard. The proposed method was validated according to the ICH guidelines and was successfully applied to the analysis of these drugs in their tablet dosage forms with high accuracy. Limits of detection were found to be 0.03, 0.07, 0.033 and 0.11 μg/mL for PAR, ACF, TZD and NMD, respectively. The high sensitivity of developed method permitted its application to the in-vitro determination of the cited drugs in spiked human plasma and urine samples, and the obtained results were satisfactory. However, PAR could not be determined in spiked human urine because its peak overlapped with that of the urine peak.

Correction to: A Micellar Liquid Chromatographic Method for the Determination of Azosemide in Solubilized System

AbstractIn the original publication of the article, the corresponding author's name was incorrectly published. The corresponding author's name should appear as Ashok Kumar.

A Micellar Liquid Chromatographic Method for the Determination of Azosemide in Solubilized System

AbstractA simple micellar liquid chromatographic method was developed and validated for the determination of azosemide (AZS). The method incorporates surfactant media beyond the critical micellar concentration level for the study of AZS in bulk and pharmaceutical dosage forms. Quantitation was achieved through UV detection. An interpretive optimization procedure was used to ascertain the optimum conditions based on the accurate description of the retention and shape of the chromatographic peak for quantification of AZS, viz., selection of surfactants, pH of buffer solution, concentration of surfactant and selection of solvent etc. The method was successfully validated as per the requirements of the international Council for Harmonisation (ICH) guidelines and showed excellent linearity within the limits of detection and limit of quantitation. The method was linear over the concentration range 0.001–0.2 mg ml−1 with regression coefficient (r2) 0.999. The proposed method was successfully applied for ascertaining the stability and determination of AZS under different stressed conditions viz., basic, acidic, oxidative, photolytic, and thermal degradation. The method elicited good selectivity, repeatability, linearity and sensitivity of the validated parameters. Recoveries obtained were in a range of 98.90–99.58%. The method allows accurate and reliable determination of AZS for drug stability assays in pharmaceutical investigations using environmentally friendly materials.

Development and validation of a micellar liquid chromatographic method to determine three antitumorals in plasma.

A micellar liquid chromatographic method to determine several anticancer drugs (pazopanib, dabrafenib and regorafenib) in plasma was developed and validated by the guidelines of the EMA. Plasma samples were directly injected, after a 1/5-dilution in a micellar solution. The drugs were resolved in <18 min using a C18 column. The mobile phase was an aqueous solution of 0.12 M SDS - 2% 1-pentanol, buffered at pH 7. The detection was performed by absorbance at 260 nm. The values of the main validation parameters were: LOD (0.1-1 mg/l), calibration range (0.2-2 to 80 mg/l), accuracy (-12.5 to +11.7%) and precision (<11.9%). The procedure was conducted by minimum cost, effort, manipulation, time and quantity of hazardous chemicals. The method was useful to determine the drugs at their respective target concentrations, and was found useful for clinical analysis.

Micellar liquid chromatographic method for the determination of ephedrine and pseudoephedrine in human serum by direct inject of the sample with simple dilution

ABSTRACTA micellar high-performance liquid chromatographic method was developed to simultaneously determine ephedrine and pseudoephedrine in human serum. The serum sample pretreatment was a simple dilution in a micellar solution, filtration, and direct injection, thus avoiding time-consuming and tedious steps. Hence, there is no need to use an internal standard. The serum samples were analyzed using a mobile phase containing 1.50 × 10−1 mol/L sodium dodecyl sulfate and 0.02 mol/L sodium dihydrogen phosphate with 7.5% (v/v) 1-propanol at pH 3.0, running at 1.0 mL/min by an Inertsil C18 (150 × 4.6 mm, 5 µm) column at 30°C. The UV wavelength was set at 210 nm. The developed method was validated by linearity (r > 0.9990) and intra- and inter-day precisions of ephedrine and pseudoephedrine (relative standard deviation; RSD%, 0.04–10.40, and RSD %, 0.30–10.25, respectively), LODs for ephedrine and for pseudoephedrine was 2.63 and 2.70 µg/mL, respectively; lower limit of quantification for ephedrine and for pseudoephedrine was 4.38 and 4.51 µg/mL, respectively. Finally, the proposed method was applied to investigate ephedrine and pseudoephedrine in real human serum samples after oral administration of Kechuanning Koufye including Ephedra herb. It is environmentally friendly, easy-to-handle, and feasible method for routine analysis in clinical laboratory.

Stability-Indicating Chromatographic Methods for Determination of Agomelatine in Drug Substance and Drug Product

Three sensitive and validated chromatographic methods were developed for determination of Agomelatine (AGO) in the presence of its degradation products in drug substance and drug product. The first and second methods were normal thin layer chromatographic (NP-TLC) and reversed phase thin layer chromatographic (RP-TLC) methods. Mobile phase consisting of ethyl acetate-ammonia (33%)-methanol (8.5:0.5:1, v/v/v) was used for NP-TLC while for RP-TLC using 0.1% triethylamine (TEA): acetonitrile (60:40 v/v) at pH=2. The chromatograms were scanned at 230 and 280 nm and determined in the range of 0.1-4 and 0.3-4 μg/spot with mean percentage recovery of 99.89 ± 1.141 and 100.01 ± 1.062 for NP-TLC and RP-TLC respectively. The third method was Micellar Liquid Chromatographic (MLC) method using C18 column and a mobile phase consisting of 0.1 M Sodium Dodecyl Sulphate (SDS), 15% butan-1-ol, 0.2% TEA in water adjusted to pH=3. The UV detection was achieved at 230 nm and determined in the range of 0.5-5 μg/mL with mean percentage recovery of 100.13 ± 0.970. The proposed methods were successfully applied as stability indicating methods under different stressed conditions according to the International Conference of Harmonization (ICH) guidelines. The methods showed good selectivity, repeatability, linearity and sensitivity according to the evaluation of the validation parameters.

Development of a gradient micellar liquid chromatographic method eluting from micellar mode to high submicellar mode for the rapid separation of free amino acids

A rapid surfactant-related gradient liquid chromatographic method progressing from a micellar liquid chromatographic mode to a submicellar liquid chromatographic mode has been developed for the quantitative analysis of free amino acids.

An ecofriendly green liquid chromatographic method for simultaneous determination of nicotinamide and clindamycin phosphate in pharmaceutical gel for acne treatment

A new green micellar liquid chromatographic method was developed and validated for the quantitative estimation of nicotinamide (NICO) and clindamycin phosphate (CLD) in bulk and pharmaceutical gel formulation. The analytes are well resolved in less than 6.0 minutes using micellar mobile phase consisting of 0.10M sodium dodecyl sulfate (SDS), 0.3% triethylamine, and 10% 2-propanol in 0.02M orthophosphoric acid at pH 3.0, running through an Eclipse XDB-C8 column (150 mm×4.6 mm, 5 μm particle size) with flow rate 1.0 mL/min. The effluent was monitored with diode array detection at 210 nm. The retention times of NICO and CLD were 3.8 minutes and 5.6 minutes, respectively. The method was validated according to the International Conference on Harmonisation (ICH) guidelines in terms of linearity, limit of detection, limit of quantification, accuracy, precision, robustness, and specificity to prove its reliability. Linear correlation was achieved by plotting the peak area of each drug against its concentration. It was found to be rectilinear in the ranges of 1.0–40.0 μg/mL and 0.5–15.0 μg/mL with limits of detection of 0.06 μg/mL and 0.03 μg/mL and limits of quantification of 0.19 μg/mL and 0.09 μg/mL for NICO and CLD, respectively. The method was successfully implemented for the simultaneous determination of the analytes in their bulk powder and combined gel formulation with high % recoveries. The ease of sample treatment facilitates and greatly expedites the treatment with reduced cost and improved accuracy of the procedure.

Rapid micellar HPLC analysis of loratadine and its major metabolite desloratadine in nano-concentration range using monolithic column and fluorometric detection: application to pharmaceuticals and biological fluids

BackgroundLoratadine is a commonly used selective non-sedating antihistaminic drug. Desloratadine is the active metabolite of loratadine and, in addition, a potential impurity in loratadine bulk powder stated by the United States Pharmacopeia as a related substance of loratadine. Published methods for the determination of both analytes suffer from limited throughput due to the time-consuming steps and tedious extraction procedures needed for the analysis of biological samples. Therefore, there is a strong demand to develop a simple rapid and sensitive analytical method that can detect and quantitate both analytes in pharmaceutical preparations and biological fluids without prior sample extraction steps.ResultsA highly-sensitive and time-saving micellar liquid chromatographic method is developed for the simultaneous determination of loratadine and desloratadine. The proposed method is the first analytical method for the determination of this mixture using a monolithic column with a mobile phase composed of 0.15 M sodium dodecyl sulfate, 10% n-Butanol and 0.3% triethylamine in 0.02 M phosphoric acid, adjusted to pH 3.5 and pumped at a flow rate of 1.2 mL/min. The eluted analytes are monitored with fluorescence detection at 440 nm after excitation at 280 nm. The developed method is linear over the concentration range of 20.0–200.0 ng/mL for both analytes. The method detection limits are 15.0 and 13.0 ng/mL and the limits of quantification are 20.0 and 18.0 ng/mL for loratadine and desloratadine, respectively. Validation of the developed method reveals an accuracy of higher than 97% and intra- and inter-day precisions with relative standard deviations not exceeding 2%.ConclusionsThe method can be successfully applied to the determination of both analytes in various matrices including pharmaceutical preparations, human urine, plasma and breast milk samples with a run-time of less than 5 min and without prior extraction procedures. The method is ideally suited for use in quality control laboratories. Moreover, it could be a simple time-saving alternative to the official pharmacopeial method for testing desloratadine as a potential impurity in loratadine bulk powder.Graphical abstractTypical chromatogram of loratadine and its major metabolite desloratadine using the proposed micellar HPLC method