Determination Of Salbutamol Research Articles

Simultaneous Spectrophotometric Determination of Salbutamol by Coupling with Diazotized 4-Aminobenzoic acid

A simple, rapid and sensitive spectrophotmetric method for trace determination of salbutamol (SAL) in aqueous solution and in pharmaceutical preparations is described. The method is based on the diazotization coupling reaction of the intended compound with 4-amino benzoic acid (ABA) in alkaline medium to form an intense orange, water soluble dye that is stable and shows maximum absorption at 410 nm. A graph of absorbance versus concentration indicates that Beer’s law is obeyed over the concentration range of 0.5-30 ppm, with a molar absorbtivity 3.76×104 L.mol-1 .cm-1 depending on the concentration of SAL. The optimum conditions and stability of the colored product have been investigated and the method was applied successfully to the determination of SAL in dosage forms.

Determination of β-agonists in Porcine Meats by Ion-Pair Extraction and High Performance Liquid Chromatography

ABSTRACTIon-paired extraction was employed for the determination of salbutamol, clenbuterol, and ractopamine. Tetrabutylammonium bromide was used as the ion-pairing agent and water–acetonitrile was the extraction solvent. The concentration and pH of the buffer, salt addition, concentration of tetrabutylammonium bromide, and type and volume of extraction solvent were optimized. No centrifugation step was required. Matrix interferences from real samples were eliminated using matrix-matched calibration. Under the optimum conditions, a linear calibration relationship was present from 0.0025 to 3 µg mL−1 with an enrichment factor of more than 25. This method was combined with high-performance liquid chromatography for the determination of β-agonists in porcine meats with low limits of detection, high recovery, and rapid analysis.

Determination of Salbutamol, Clenbuterol, and Brombuterol in Urine by a Highly Sensitive Chemiluminescence Enzyme Immunoassay

A salbutamol-bovine serum albumin and a salbutamol-ovalbumin coating antigen were synthesized, and six New Zealand white rabbits were treated with the immunogen to obtain polyclonal antibodies to develop a rapid, sensitive, and indirect chemiluminescent enzyme immunoassay (ciCLEIA) for the analysis of swine and bovine urine. The prepared antibodies showed high cross-reactivities with clenbuterol (139.6%) and brombuterol (225%). Under the optimized conditions, the linear dynamic range and the limit of detection (LOD) for salbutamol were from 0.007 to 0.17 µg L−1 and 0.003 µg L−1, with a correlation coefficient of 0.9965 and a half maximum inhibition concentration of 0.028 µg L−1. Recoveries for salbutamol, clenbuterol, and brombuterol were from 78.8% to 119.0% with intra-assay and inter-assay coefficients of variation less than 13.9% and 19.7%, respectively. The reported ciCLEIA was about 10-fold more sensitive for salbutamol and 20-fold more sensitive for clenbuterol compared to conventional methods. This study showed that ciCLEIA was a reliable, convenient, and sensitive method for the simultaneous determination of salbutamol, clenbuterol, and brombuterol in swine and bovine urine.

Matrix effects in the determination of β‐receptor agonists in animal‐derived foodstuffs by ultra‐performance liquid chromatography tandem mass spectrometry with immunoaffinity solid‐phase extraction

Matrix effects in determination of three β-receptor agonists including salbutamol (SAL), clenbuterol, and terbutaline in animal-derived foodstuffs were studied by ultra-performance LC-MS/MS with cleanup of immunoaffinity SPE column (IAC). Some animal tissue samples including pig liver, swine muscle, and fish muscle were hydrolyzed by the mixed enzyme solution or HCl solution, and the cleanup efficiencies with SAL IAC, MCX SPE column, and C(18) -SCX tandem columns were examined and compared by using spiked experiments. The results showed that the matrix effects in the determination of SAL and terbutaline can be eliminated with SAL IAC cleanup, and the average recoveries of SAL were 77.4~81.5%, 79.0~80.3%, and 85.0~87.2% in pig liver, swine muscle, and fish muscle, respectively. The decision limit (ccα) and detection capability (ccβ) for SAL in pig liver were 0.02 and 0.05 μg/kg, respectively.

Capillary Electrophoresis Coupled with Electrochemiluminescence for the Facile Separation and Determination of Salbutamol and Clenbuterol in Urine

AbstractA capillary electrophoresis coupled with tris(2,2′‐bipyridyl) ruthenium(II) (Ru(bpy)32+) electrochemiluminescence detection system was developed to determine salbutamol and clenbuterol in urine. Some factors that affected the performances of separation and detection were investigated. Under the optimized conditions, one single quantitative analysis of salbutamol and clenbuterol was achieved at a separation voltage of 15 kV within 9 min, and the LODs (S/N=3) and LOQs (S/N=10) of salbutamol and clenbuterol were 8.43×10−8 mol/L, 2.61×10−7 mol/L and 2.73×10−7 mol/L, 8.21×10−7 mol/L, respectively. The recovery obtained from the analysis of spiked urine samples was between 88.6 % and 104.7 % with RSDs lower than 6.70 %. The method was successfully applied to determine salbutamol and clenbuterol in urine samples.

Determination of salbutamol and salbutamol glucuronide in human urine by means of liquid chromatography‐tandem mass spectrometry

The determination of salbutamol and its glucuronide in human urine following the inhalative and oral administration of therapeutic doses of salbutamol preparations was performed by means of direct urine injection utilizing liquid chromatography-tandem mass spectrometry (LC-MS/MS) and employing d(3)-salbutamol and d(3)-salbutamol glucuronide as internal standards. Unconjugated salbutamol was detected in all administration study urine samples. Salbutamol concentrations following inhalation were commonly (99%) below 1000 ng/ml whereas values after oral administration frequently (48%) exceeded this threshold. While salbutamol glucuronide was not detected in urine samples collected after inhalation of the drug, 26 out of 82 specimens obtained after oral application contained salbutamol glucuronide with a peak value of 63 ng/ml. The percentage of salbutamol glucuronide compared to unconjugated salbutamol was less than 3%. Authentic doping control urine samples indicating screening results for salbutamol less than 1000 ng/ml, showed salbutamol glucuronide concentrations between 2 and 6 ng/ml, whereas adverse analytical findings resulting from salbutamol levels higher than 1000 ng/ml, had salbutamol glucuronide values between 8 and 15 ng/ml. The approach enabled the rapid determination of salbutamol and its glucuronic acid conjugate in human urine and represents an alternative to existing procedures since time-consuming hydrolysis or derivatization steps were omitted. Moreover, the excretion of salbutamol glucuronide in human urine following the administration of salbutamol was proven.

Determination of salbutamol in human plasma and urine by gas chromatography—mass spectrometry

Determination of salbutamol in human plasma and urine by gas chromatography—mass spectrometry

Sensitive Micellar Electrokinetic Chromatographic Determination of Salbutamol, Guaifenesin, and Dyphylline in Oral Formulations

A sensitive micellar electrokinetic chromatographic method to analyze salbutamol, guaifenesin, and dyphylline employing 20 µm inner diameter capillaries was developed. Sensitive analysis of the drugs at a concentration range of about 0.5 to 60 µg/mL was demonstrated using large volume sample stacking with 75% acetonitrile as the sample diluent. Using dyphylline as the internal standard, detection limits were 0.07 µg/mL and 0.21 µg/mL for salbutamol and guaifenesin, respectively. Using the standard addition method, accurate determination of salbutamol and guaifenesin in syrup and capsule preparations was achieved. Recovery values were satisfactory (95 to 100%), but matrix interferences affected the reproducibility.

Effect of graphite and metallic impurities of C 60 fullerene on determination of salbutamol in biological fluids

A new method for the determination of salbutamol has been developed using fullerene C 60-modified glassy carbon electrode and validated using GC–MS. The presence of graphite and metallic impurities in C 60 are found to diminish the peak. The oxidation of salbutamol was observed in a single well-defined, diffusion-controlled process using square wave voltammetry. The peak potential of oxidation peak was dependent on pH and determination was carried out at physiological pH 7.4. The peak current versus concentration plot was linear in the range 100–2000 ng/ml of salbutamol. The detection limit was found to be 40 ng/ml. The determination of salbutamol was carried out in human blood and urine samples and common interferents such as dopamine, ascorbic acid and uric acid do not interfere. The method proved to be specific, rapid, and accurate and can be easily applied for detecting cases of doping. A cross-validation of the observed results with GC–MS indicated a good agreement.

Immunoaffinity chromatography for purification of Salbutamol and Clenbuterol followed screening and confirmation by ELISA and GC-MS

Screening and confirmatory methods for the determination of Salbutamol (SAL) and Clenbuterol (CL) in swine urine were established. The polyclonal antibody against SAL was prepared, which was used to develop the indirect competitive enzyme-linked immunosorbent assay (ELISA) with the limit of detection of 0.5 ng/ml, and to prepare the immunoaffinity chromatography column. The immunoaffinity column could extract and purify SAL and CL simultaneously, with a binding capacity of 400 ng for SAL and 416 ng for CL. After purification, the swine urine samples were screened by ELISA for the presence of SAL and/or CL, and the positive samples were further confirmed and quantified by gas chromatography-mass spectrometry (GC-MS). The results showed that 95% of the positive samples were confirmed by GC-MS with various levels of SAL (1.1–4.6 ng/ml) and/or CL (1.9–229.1 ng/ml) residues in the incurred samples, and all the negative samples were confirmed with no SAL and/or CL residues.

Determination of salbutamol in syrups by capillary electrophoresis with contactless conductivity detection (CE-C 4D)

This paper describes the separation and quantification of salbutamol in pharmaceutical products (salbutamol syrups) by capillary electrophoresis (CE) with contactless conductivity detection (C 4D). The system was studied by micellar electrokinetic capillary chromatography (MEKC) and free solution capillary electrophoresis (FSCE), being the latter chosen in function of best resolution and sensitivity in comparison with the MEKC method. CE-C 4D was applied to analysis of salbutamol in syrups utilizing 1.0 × 10 −2 mol L −1 acetic acid/sodium acetate buffer (pH 4.9) as running electrolyte. Tetraethylammonium (TEA) solution was used as internal standard. The results obtained include a linear dynamic range from 7.0 × 10 −5 to 3.0 × 10 −4 mol L −1 and good repeatability (R.S.D. = 4.7% for n = 10 for a 7.0 × 10 −5 mol L −1 salbutamol solution). The detection limit was calculated as 1.0 × 10 −5 mol L −1 and the limit of quantification was estimated as 3.3 × 10 −5 mol L −1. For syrups analysis the reproducibility presented deviations between 1.5% and 2.5% (three different days) obtained for measurements in triplicate.

Determination of Salbutamol in Pharmaceuticals by Capillary Electrophoresis

A capillary electrophoresis (CE) method for the separation and determination of salbutamol (SAL) in commercial pharmaceuticals was developed. Several parameters affecting the separations were studied including type and concentration of the carrier ion, counter ion, and the pH of the buffer. A hydrodynamically closed CE separation mode employing a 300 mum I.D. capillary, dynamically coated by polymeric buffer additive, provided good performance parameters (precision, accuracy, sensitivity). The obtained results suggest that the proposed method is suitable for routine assay of SAL in pharmaceutical preparations and can be used as an alternative to the conventional open CE mode for this application.

Clean-up, detection and determination of salbutamol in human urine and serum

Salbutamol ¿2-(tert-butylamino)-1-[4-hydroxy-3- (hydroxymethyl)phenyl]ethanol¿, also known as albuterol, is clinically the most widely used beta 2-adrenoceptor agonist in the treatment of bronchial asthma. During this study, we evaluated liquid-liquid extraction (LLE) and solid-phase extraction (SPE) in order to develop a reliable extraction method followed by analysis using liquid chromatography and gas chromatography. An assay is described which involves SPE as the clean-up method followed by gas chromatography-mass spectrometry to determine salbutamol levels in human serum after oral administration. The SPE method requires the use of a hyper-cross-linked styrene-divinylbenzene bonded phase (ENV+) without involving any sample pre-treatment to obtain 60-65% recoveries for salbutamol and terbutaline as the internal standard. Distilled water and 1% trifluoroacetic acid in methanol were found to be the most suitable washing solvent and eluting solvent, respectively. A detection limit of 2 ng mL-1 was achieved by derivatization with N-methyl-N-trimethylsilyltrifluoroacetamide to form trimethylsilyl (TMS)-salbutamol (m/z 369) and TMS-terbutaline (m/z 356). The relationship between the ratio of the peak area of salbutamol to that of the internal standard and concentration was linear for the range tested (2-200 ng mL-1) and the correlation of coefficient was 0.9999 with a y-intercept not significantly different from zero. The inter-day relative standard deviation (RSD) was < 10% for all three concentrations. The intra-day RSD was 14% for 2 ng mL-1. This assay was then successfully applied to human serum samples obtained from clinical trials after oral administration of salbutamol.

Electrokinetic behaviour of salbutamol and its decomposition products and determination of salbutamol by micellar electrokinetic capillary chromatography

Separation in capillary electrophoresis is governed by several factors, including type of buffer, buffer concentration, pH, temperature, voltage and micelles. Through proper adjustment of these parameters, salbutamol could be separated from its acidic and basic decomposition products. The determination of salbutamol in kinetic studies was achieved by micellar electrokinetic capillary chromatography (MECC) using a mixture of N-cetyl-N,N,N-trimethylammonium bromide (5 m M), disodium hydrogenphosphate (20 m M) and sodium tetraborate (20 m M) (pH 7.6) with phosphoric acid. The MECC results were in good agreement with results obtained by high-performance liquid chromatography.

Validation of a method for the determination of salbutamol in animal urine by gas chromatography-mass spectrometry and its application to treated lamb samples

Validation of a method for the determination of salbutamol in animal urine by gas chromatography-mass spectrometry and its application to treated lamb samples

Determination of salbutamol in plasma by high-performance liquid chromatography with fluorescence detection

Determination of salbutamol in plasma by high-performance liquid chromatography with fluorescence detection