Application of Chemometrics-assisted HPLC-DAD Strategies for Simultaneous Determination of Paracetamol, Pseudoephedrine HCl, Dextromethorphan HBr, Doxylamine Succinate and Saccharin in Syrup Formulation

2020 ◽  
Vol 16 ◽  
Author(s):  
Abdürrezzak E. Bozdoğana ◽  
Özlem Aksu Dönmez ◽  
Şule Dinç-Zor
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Multivariate Calibration ◽  
Low Cost ◽  
Pharmaceutical Products ◽  
Complete Separation ◽  
Target Analytes ◽  
Calibration Methods ◽  
Array Detection

Introduction: This study introduces an effective strategy which combines high performance liquid chromatography coupled with diode array detection (HPLC-DAD) with multivariate calibration methods for the simultaneous determination paracetamol (PAR), pseudoephedrine HCl (PSE), dextromethorphan HBr (DEX) and doxylamine succinate (DOX) along with sweetener saccharine (SAC) in syrup formulation. Methods: PLS-2 and PCR calibration algorithms were selected for data processing. Based on the strategy, all target analytes were rapidly quantified within 5.3 min under the simple isocratic elution (water : methanol, 20/80, v/v) without a complete separation. The performances of the proposed methods were confirmed by analyzing a series of synthetic solutions including different concentrations of analytes Results: The average recovery values were in the range of 100.33 to 103.70%, and the REP (relative error of prediction) values ranged from 1.96 to 4.36% showed that these methods could provide satisfactory predictions. Conclusion: Novel HPLC methods coupled with PLS and PCR algorithm enable a simple, fast and low-cost analysis of similar pharmaceutical products for simultaneous determination of the target compounds.

scholarly journals Development and Validation of HPLC-DAD Method for Simultaneous Determination of Seven Food Additives and Caffeine in Powdered Drinks

Foods ◽  
2020 ◽  
Vol 9 (8) ◽  
pp. 1119
Author(s):  
Imanulkhan Imanulkhan ◽  
Widiastuti Setyaningsih ◽  
Abdul Rohman ◽  
Miguel Palma
Keyword(s):  
Simultaneous Determination ◽  
Phosphate Buffer ◽  
High Performance ◽  
Desirability Function ◽  
Food Additives ◽  
Complete Separation ◽  
Sodium Saccharin ◽  
Array Detection ◽  
Development And Validation

The usage of food additives must respect the general legislation in force in the country and requires a reliable analytical method for surveillance. This research aimed to develop a high-performance liquid chromatography with diode array detection (HPLC-DAD) method for the simultaneous determination of seven food additives and caffeine in powdered drinks. Three factors likely to affect the chromatographic separation, namely, mobile phase composition at the beginning (x1, 0–10% of the amount of methanol in the phosphate buffer) and the end (x2, 60–100% of the amount of methanol in the phosphate buffer) of the gradient program and pH (x3, 3–7), were evaluated with the aid of a Box–Behnken Design (BBD). Subsequently, multi-response optimizations for chromatographic resolutions (Rs) and analysis time were performed using the response surface methodology (RSM) in conjunction with the desirability function (DF). Complete separation (Rs > 1.5) of seven food additives and caffeine was achieved in less than 16 min by applying 8.5% methanol in the phosphate buffer at the beginning and 90% at the end of the gradient program, in pH 6.7. The developed method was validated with low limits of detection (ranging from 1.16 mg kg−1 (sodium saccharin) to 3.00 mg kg−1 (acesulfame potassium)), low limits of quantification (ranging from 3.86 mg kg−1 (sodium saccharin) to 10.02 mg kg−1 (acesulfame potassium)), high precision (CV < 4%), and high accuracy (recoveries from 95 to 101% at 80, 100, and 120% of the target concentration). The method was successfully used to assess the seven food additives and caffeine in commercially available powdered drinks.

scholarly journals Simultaneous Determination of Chlorthalidone and Spironolactone with Univariate and Multivariate Calibration: Wavelength Range Selection

1999 ◽  
Vol 82 (5) ◽  
pp. 1054-1063 ◽  
Author(s):  
M Luz Luis ◽  
José M García ◽  
Francisco Jiménez ◽  
Ana I Jiménez ◽  
Juan J Arias
Keyword(s):  
Simultaneous Determination ◽  
Wavelength Range ◽  
High Performance ◽  
Multivariate Calibration ◽  
Pharmaceutical Preparation ◽  
Least Squares Regression ◽  
Zero Crossing ◽  
Number Of Factors ◽  
Calibration Methods

Abstract Chlorthalidone and spironolactone were determined simultaneously with the aid of univariate and multivariate calibration methods. Univariate calibration was performed by the zero-crossing and derivative ratio spectrum methods. Extensive spectral overlap and the scarcity of wavelengths in derivative spectra allowing one analyte to be distinguished and quantitated in the presence of the other gave rise to poor results that called for multivariate calibration. Partial least-squares regression was used in combination with a suitable method for selecting the optimum wavelength range and number of factors for analysis. The ensuing method was applied to simultaneous determination of chlorthalidone and spironolactone in a commercially available pharmaceutical preparation. The results were validated by high-performance liquid chromatography.

Solvent bar microextraction combined with HPLC-DAD for simultaneous determination of diuretics in human urine and plasma samples

2021 ◽  
Vol 22 ◽  
Author(s):  
Nabil N. AL-Hashimi ◽  
Amjad H. El-Sheikh ◽  
Manal I. Alruwad ◽  
Mohanad M. Odeh
Keyword(s):  
Simultaneous Determination ◽  
Human Urine ◽  
High Performance ◽  
Plasma Samples ◽  
Satisfactory Precision ◽  
Array Detection ◽  
Spiked Human Urine ◽  
Analytical Technology ◽  
Solvent Bar Microextraction

Background: A simple and powerful microextraction procedure, the solvent bar microextraction (SBME), was used for the simultaneous determination of two diuretics, furosemide and spironolactone in human urine and plasma samples, using high-performance liquid chromatography coupled with diode array detection (HPLC-DAD). Methods: The appropriate amount (2 µL) of 1-octanol as an organic solvent confined within (2.5 cm) of a porous hollow fiber micro-tube, sealed at both ends was used for this procedure. The conditions for the SBME were optimized in water and the analytical performance were examined in spiked human urine and plasma samples. Results: The optimized method exhibited good linearity (R2 > 0.997) over the studied range of higher than 33 to 104 µg L-1 for furosemide and spironolactone in urine and plasma samples, illustrating a satisfactory precision level with RSD values between 2.1% and 9.1%. Discussion: The values of the limits of detection were found to be in the range of 6.39 to 9.67 µg L-1, and extraction recovery˃ 58.8% for both diuretics in urine and plasma samples. The applicability and effectiveness of the proposed method for the determination of furosemide and spironolactone in patient urine samples were tested. Conclusion: In comparison with reference methods, the attained results demonstrated that SBME combined with HPLC-DAD was proved to be simple, inexpensive, and promising analytical technology for the simultaneous determination of furosemide and spironolactone in urine and plasma samples.

Environmentally Evaluated New HPLC/UV Method for the Simultaneous Determination of Acesulfame-K, Butylated Hydroxytoluene, and Aspartame and Its Degradant in Chewing Gum

2019 ◽  
Vol 102 (6) ◽  
pp. 1892-1900
Author(s):  
Nada S. Zamzam ◽  
Mona H. Abdel Rahman ◽  
Maha F. Abdel Ghani
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Low Cost ◽  
Food Additives ◽  
Gradient Elution ◽  
Butylated Hydroxytoluene ◽  
Chewing Gum ◽  
Adverse Health Effects ◽  
Chewing Gums

Background: Acesulfame-K (ACE), butylated hydroxytoluene (BHT), and aspartame (ASP) are a common combination of food additives added to chewing gums. The abuse of these additives results in severe adverse health effects; however, they are still extensively used owing to their high performance and low cost. Objective: The development and optimization of a simple, cheap, sensitive, and eco-friendly HPLC/UV method for the simultaneous determination of ASP, ACE, and BHT along with aspartame degradation product phenylalanine (PHEN) in chewing gum. Methods: The method was optimized using a 5 μm C18 column and an eluent consisting of methanol and 0.1 M phosphate buffer (pH 5.0) according to a suitable gradient elution program. Simple sample preparation, consisting of dilution, homogenization, and sonication followed by centrifugation and filtration, was optimized and used for the extraction of chewing gum. The greenness of the method was evaluated. Results: The proposed method exhibited excellent linearity (R2 > 0.9996), low LOQ (0.08–0.95 μg/mL), and recoveries between 85.3 and 98.83% with relative SD (RSD) ≤ 2.7%. High resolution was obtained with <25 min run times with excellent precision (RSD: 0.28–1.33%). This method was successfully applied for the simultaneous determination of ACE, ASP, and BHT in commercial chewing gum; PHEN was not detected. Furthermore, our method is considered to be environmentally acceptable. Conclusions: The results demonstrate that the developed method can be used to detect ACE, BHT, ASP, and PHEN in chewing gum. Highlights: A new sensitive, green HPLC/UV method is developed to be used as a minimal-cost routine analysis procedure for commercial chewing gum.

Environmentally Evaluated New HPLC/UV Method for the Simultaneous Determination of Acesulfame-K, Butylated Hydroxytoluene, and Aspartame and Its Degradant in Chewing Gum

2019 ◽  
Vol 102 (6) ◽  
pp. 1892-1900
Author(s):  
Nada S Zamzam ◽  
Mona H Abdel Rahman ◽  
Maha F Abdel Ghani
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Low Cost ◽  
Food Additives ◽  
Gradient Elution ◽  
Butylated Hydroxytoluene ◽  
Chewing Gum ◽  
Adverse Health Effects ◽  
Chewing Gums

Abstract Background: Acesulfame-K (ACE), butylated hydroxytoluene (BHT), and aspartame (ASP) are a common combination of food additives added to chewing gums. The abuse of these additives results in severe adverse health effects; however, they are still extensively used owing to their high performance and low cost. Objective: The development and optimization of a simple, cheap, sensitive, and eco-friendly HPLC/UV method for the simultaneous determination of ASP, ACE, and BHT along with aspartame degradation product phenylalanine (PHEN) in chewing gum. Methods: The method was optimized using a 5 μm C18 column and an eluent consisting of methanol and 0.1 M phosphate buffer (pH 5.0) according to a suitable gradient elution program. Simple sample preparation, consisting of dilution, homogenization, and sonication followed by centrifugation and filtration, was optimized and used for the extraction of chewing gum. The greenness of the method was evaluated. Results: The proposed method exhibited excellent linearity (R2 &gt; 0.9996), low LOQ (0.08–0.95 μg/mL), and recoveries between 85.3 and 98.83% with relative SD (RSD) ≤ 2.7%. High resolution was obtained with &lt;25 min run times with excellent precision (RSD: 0.28–1.33%). This method was successfully applied for the simultaneous determination of ACE, ASP, and BHT in commercial chewing gum; PHEN was not detected. Furthermore, our method is considered to be environmentally acceptable. Conclusions: The results demonstrate that the developed method can be used to detect ACE, BHT, ASP, and PHEN in chewing gum. Highlights: A new sensitive, green HPLC/UV method is developed to be used as a minimal-cost routine analysis procedure for commercial chewing gum.

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