A New Application of PARAFAC Model to UPLC Dataset for the Quantitative Resolution of a Tri-Component Drug Mixture

2021 ◽  
Author(s):  
Remziye Güzel ◽  
Zehra Ceren Ertekin ◽  
Erdal Dinç
Keyword(s):  
Quantitative Estimation ◽  
Pharmaceutical Preparation ◽  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
Ultra Performance Liquid Chromatography ◽  
Parafac Model ◽  
Independent Test ◽  
Photodiode Array ◽  
Parallel Factor ◽  
Parafac Decomposition

Abstract In the presented work, a three-way analysis of ultra-performance liquid chromatography-photodiode array (UPLC-PDA) dataset was performed by parallel factor analysis (PARAFAC) for quantitatively resolving a ternary mixture containing paracetamol and methocarbamol with indapamide selected as an internal standard in their co-eluted chromatographic conditions. Paracetamol and methocarbamol were quantified in the working range between 3–24 and 5–50 μg/mL by applying PARAFAC decomposition to UPLC-PDA data array obtained under unresolved chromatographic peak conditions. To compare the experimental results provided by co-eluted UPLC-PARAFAC method, an ordinary UPLC method was developed ensuring proper separation of the peaks. The performance of both PARAFAC and ordinary UPLC methods were assessed by quantifying independent test samples, intra- and inter-day samples and spiked samples of pharmaceutical preparations. Then, both methods were applied for quantitative estimation of the related drugs in a commercial pharmaceutical preparation. In this study, PARAFAC method was proved to be a very powerful alternative for the quality control of pharmaceutical preparations containing paracetamol and methocarbamol even in their co-eluted chromatograms with high precision and accuracy in a short chromatographic runtime of 1.2 min.

scholarly journals Development and Validation of Spectrophotometric and High-Performance Column Liquid Chromatographic Methods for the Simultaneous Determination of Dienogest and Estradiol Valerate in Pharmaceutical Preparations

2010 ◽  
Vol 93 (3) ◽  
pp. 862-868 ◽  
Author(s):  
Mehmet Gökhan Çağlayan ◽  
Ismail Murat Palabiyik ◽  
Feyyaz Onur
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Pharmaceutical Preparation ◽  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
Principal Component ◽  
Data Matrix ◽  
Estradiol Valerate ◽  
Concentration Data

Abstract Simultaneous determination of dienogest (DIE) and estradiol valerate (EST) in sugar-coated tablets was performed by using HPLC and spectrophotometry. In HPLC, the separation was achieved on an ACE C8 column using the mobile phase acetonitrileNH4NO3 (0.03 M, pH 5.4; 70 + 30, v/v) at a flow rate of 2 mL/min. The detection wavelength was 280 nm, and cyproterone acetate was selected as an internal standard. The linearity range was 3.045.0 g/mL for DIE and 18.0100.0 g/mL for EST. As spectrophotometric methods, two chemometric methods, principal component regression and partial least-squares, were developed. In the chemometric techniques, the concentration data matrix was prepared by using mixtures containing these drugs in methanolwater (3 + 1, v/v). The absorbance data matrix corresponding to the concentration data matrix in these methods was obtained by the measurement of absorbances in their zero-order spectra; then, the calibration was obtained by using the data matrix for the prediction of unknown concentrations of DIE and EST in their binary mixture. Working ranges were found as 2.024.0 g/mL for DIE and 20.0270.0 g/mL EST in the methods. These three developed methods were validated and successfully applied to a pharmaceutical preparation, a sugar-coated tablet, and the results were compared with each other.

Development and Validation of Novel UPLC-MS/MS Method for the Analysis of Macitentan in Pharmaceutical Formulations

2019 ◽  
Vol 15 (5) ◽  
pp. 554-559
Author(s):  
Mevlut Albayrak ◽  
Alptug Atila
Keyword(s):  
Atmospheric Pressure Chemical Ionization ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Ultra Performance Liquid Chromatography ◽  
Pure Form ◽  
Column Temperature ◽  
Limit Of Quantitation

Introduction: Macitentan is an endothelin receptor antagonist drug used in the treatment of pulmonary arterial hypertension. Materials and Methods: A new, sensitive, simple, accurate and rapid ultra-performance liquid chromatography in combination with tandem triple quadruple mass spectrometry (UPLC-MS/MS) method has been developed and validated for the determination of macitentan in pharmaceutical formulations. Macitentan and bosentan which are used as internal standard (IS) were detected using atmospheric pressure chemical ionization (APCI) in positive ion, multiple reaction monitoring (MRM) mode by monitoring mass transitions (precursor to product) m/z 589.1→203.3 and 552.6→311.5, respectively. Chromatographic separation was carried out on reverse phase C18 column (5 µm, 4.6 * 150 mm). Water containing 0.2 % acetic acid in acetonitrile (10:90, v/v) was used as the mobile phase in the isocratic elution. The system was optimized with injection volume of 10 µL, column temperature of 35 °C and flow rate of 1 mL min-1 Retention times were 1.97 min for macitentan and 1.72 min for IS. Results and Discussion: The calibration curve with a high correlation coefficient (0.9997) was linear range 0.5-500 ng mL-1. The lower limit of quantitation (LLOQ) and average recovery values were determined as 0.5 ng mL-1 and 99.7 %, respectively. The developed novel method has been successfully applied for the determination of macitentan in pure form and pharmaceutical formulations. Conclusion: The present method is the first study developed and validated for the determination of macitentan from the pharmaceutical preparations and pure form by UPLC-MS/MS method in the literature.

A novel and sensitive LC-MS/MS method for the quantitation of ceftiofur in pharmaceutical preparations and milk samples

2020 ◽  
Vol 23 ◽  
Author(s):  
Serkan Levent ◽  
Saniye Özcan ◽  
Aysun Geven ◽  
Nafiz Öncü Can
Keyword(s):  
Quantitative Estimation ◽  
Signal To Noise Ratio ◽  
Multiple Reaction Monitoring ◽  
Pharmaceutical Preparations ◽  
Calibration Method ◽  
Negative Ion ◽  
Cow Milk ◽  
Tandem Mass ◽  
Ionization Source ◽  
Liquid Chromatography Tandem Mass

Introduction:: In the present study, a sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was described for the determination of ceftiofur (CEF) in cow milk and pharmaceutical preparations. CEF is an antibiotic compound, which is commonly used in the treatment of animal diseases such as respiratory system, soft tissue, and foot infections, as well as postpartum acute puerperal metritis. One of the critical features of CEF is its prescription while breastfeeding of cows; in accordance, its quantitative estimation is essential to assess its residual amounts. Methods:: In the method reported herein, after simple protein precipitation using acetonitrile, the pre-treated samples were introduced in to an LC-MS/MS instrument equipped with a Chromolith® High-Resolution RP-18 series HPLC column (100 mm × 4.6 mm from Merck KGaA, Germany). Electrospray ionization was employed as the ionization source in the triplequadrupole tandem mass spectrometer. Results:: For the calibration method using solvent-based standards; LOQ was 3.038 ng/mL, 12.15 ng/mL, and LOD was 1.215 ng/mL and 6.076 ng/mL for ESI+ and ESI- modes, respectively. On the other hand, for the method of matrix-matched standards; LOQ was 1.701 ng/mL, 10.13 ng/mL, and LOD was 0.486 ng/mL and 5.929 ng/mL for ESI+ and ESI- modes, respectively as obtained from signal to noise ratio. Conclusion:: Applicability of both positive and negative ion modes was tested, and the analyte was detected via multiple reaction monitoring. The distorting effects of the milk matrix on the MS ionization and quantitation of CEF were overcome by using matrix-matched calibration for the first time.

Simultaneous Determination of Methocarbamol and Paracetamol in the Presence of Three Related Substances by Ultra Performance Liquid Chromatography

2019 ◽  
Vol 15 (5) ◽  
pp. 505-510
Author(s):  
Yanjuan Zheng ◽  
Qiushi Peng ◽  
Rui Dong ◽  
Tingyu Chen ◽  
Yi Bao ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Pharmaceutical Preparations ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Related Substances ◽  
Bulk Powder ◽  
Highly Sensitive ◽  
Optimal Protocol ◽  
Acquity Uplc

Introduction: A rapid, and accurate Ultra Performance Liquid Chromatography (UPLC) method was developed to simultaneously analyze Methocarbamol, Paracetamol and the related substances Materials and Methods: Waters ACQUITY UPLC® BEH Phenyl C18 column was used in conjunction with UV detection at 225nm. Gradient elution with 0.05M, pH 6 phosphate buffer and acetonitrile flow at 0.3mL /min rate were used to separate the substances. The retention times for 4-Aminopheno, Paracetamol, Guaifenesin, Methocarbamol, and 4-Chloroacetanilide were 1.319 minute, 2.224 minute, 4.467 minute, 4.769 minute and 5.433 minute respectively. The concentration was linear in the range of 2-100 µg/ml for Methocarbamol, and 1-100 µg/mL for Paracetamol. The percentage recoveries were between 99.28±1.23% to 100.57±0.99% for Methocarbamol, and between 99.08±1.23% to 101.23±1.39% for Paracetamol. Results and Discussion: The validated optimal protocol is robust and accurate for simultaneous analysis of Methocarbamol, Paracetamol and the related substances, applicable for bulk powder as well as pharmaceutical formulation. Conclusion: In this paper, a highly sensitive, accurate, and precise UPLC method with UV-Vis detection was developed and validated for quality control of MET and PAR in bulk as well as in pharmaceutical preparations.

Simultaneous Determination of Alogliptin, Linagliptin, Saxagliptin, and Sitagliptin in Bulk Drug and Formulation by UPLC Q-TOF-MS

2020 ◽  
Vol 17 (1) ◽  
pp. 95-105
Author(s):  
Ramji Rathod ◽  
Faraat Ali ◽  
Amrish Chandra ◽  
Robin Kumar ◽  
Meenakshi Dahiya ◽  
...  
Keyword(s):  
Internal Standard ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Pharmaceutical Dosage Forms ◽  
Sensitivity And Selectivity ◽  
The Mean ◽  
Bulk Drug ◽  
Positive Ion ◽  
Higher Sensitivity

Background: A simple and sensitive Ultra Performance Liquid Chromatography-Mass Spectrometry method was developed and validated to measure the concentrations of Alogliptin (ALO), Linagliptin (LIN), Saxagliptin (SAX), and Sitagliptin (SIT) using Pioglitazone (PIO) as an internal standard. Methods: Chromatographic separation of six gliptins was achieved on a C-18 column (100×2.1 mm, 2.7 μm) using a mobile phase consisting of formic acid in water, 0.1%v/v: acetonitrile in gradient elution. Electrospray ionization (ESI) source was operated in the positive ion mode. Targeted MS/MS mode on a QTOF MS was used to quantify the drug utilizing the transitions of 340.1(m/z), 473.2 (m/z), 316.2 (m/z), 408.1 (m/z), and 357.1 (m/z) for ALO, LIN, SAX, SIT and PIO respectively. Results: As per ICH Q2R1 guidelines, a detailed validation of the method was carried out and the standard curves were found to be linear over the concentration ranges of 1516.0-4548.1 ng mL-1, 519.8- 1559.4 ng mL-1, 1531.4-4594.3 ng mL-1and 1519.6-4558.8 ng mL-1 for ALO, LIN, SAX and SIT respectively. Precision and accuracy results were within the acceptable limits. The mean recovery was found to be 98.8 _ 0.76 % (GEM), 102.2 _ 1.59 % (LIN), 95.3 _ 2.74 % (SAX) and 99.2 _ 1.75 % (SIT) respectively. Conclusions: The optimized validated UPLC QTOF-MS/MS method offered the advantage of shorter analytical times and higher sensitivity and selectivity. The optimized method is suitable for application in quantitative analysis of pharmaceutical dosage forms for QC laboratory.

scholarly journals Angle Estimation for MIMO Radar in the Presence of Gain-Phase Errors with One Instrumental Tx/Rx Sensor: A Theoretical and Numerical Study

2021 ◽  
Vol 13 (15) ◽  
pp. 2964
Author(s):  
Fangqing Wen ◽  
Junpeng Shi ◽  
Xinhai Wang ◽  
Lin Wang
Keyword(s):  
Numerical Study ◽  
Multiple Input Multiple Output ◽  
Mimo Radar ◽  
Phase Errors ◽  
Direction Of Departure ◽  
Multiple Input ◽  
Input Multiple Output ◽  
Angle Pair ◽  
Parallel Factor ◽  
Parafac Decomposition

Ideal transmitting and receiving (Tx/Rx) array response is always desirable in multiple-input multiple-output (MIMO) radar. In practice, nevertheless, Tx/Rx arrays may be susceptible to unknown gain-phase errors (GPE) and yield seriously decreased positioning accuracy. This paper focuses on the direction-of-departure (DOD) and direction-of-arrival (DOA) problem in bistatic MIMO radar with unknown gain-phase errors (GPE). A novel parallel factor (PARAFAC) estimator is proposed. The factor matrices containing DOD and DOA are firstly obtained via PARAFAC decomposition. One DOD-DOA pair estimation is then accomplished from the spectrum searching. Thereafter, the remainder DOD and DOA are achieved by the least squares technique with the previous estimated angle pair. The proposed estimator is analyzed in detail. It only requires one instrumental Tx/Rx sensor, and it outperforms the state-of-the-art algorithms. Numerical simulations verify the theoretical advantages.

scholarly journals An Accurate and Effective Method for Measuring Osimertinib by UPLC-TOF-MS and Its Pharmacokinetic Study in Rats

Molecules ◽  
2018 ◽  
Vol 23 (11) ◽  
pp. 2894 ◽  
Author(s):  
Song-Tao Dong ◽  
Ying Li ◽  
Hao-Tian Yang ◽  
Yin Wu ◽  
Ya-Jing Li ◽  
...  
Keyword(s):  
Matrix Effects ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Rat Plasma ◽  
Analysis Method ◽  
T790m Mutation ◽  
Flight Mass Spectrometry ◽  
Relative Standard ◽  
New Generation ◽  
Tof Ms

Osimertinib, a new-generation inhibitor of the epidermal growth factor, has been used for the clinical treatment of advanced T790M mutation-positive tumors. In this research, an original analysis method was established for the quantification of osimertinib by ultra-performance liquid chromatography with time of flight mass spectrometry (UPLC-TOF-MS) in rat plasma. After protein precipitation with acetonitrile and sorafinib (internal standard, IS), they were chromatographed through a Waters XTerra MS C18 column. The mobile phase was acetonitrile and water (including 0.1% ammonia). The relative standard deviation (RSD) of the intra- and inter-day results ranged from 5.38 to 9.76% and from 6.02 to 9.46%, respectively, and the extraction recovery and matrix effects were calculated to range from 84.31 to 96.14% and from 91.46 to 97.18%, respectively. The results illustrated that the analysis method had sufficient specificity, accuracy and precision. Meanwhile, the UPLC-TOF-MS method for osimertinib was successfully applied into the pharmacokinetics of SD rats.

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