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.

A Novel Validated Ultra-Performance Liquid Chromatography Method for Separation of Eszopiclone Impurities and its Degradants in Drug Products

2013 ◽  
Vol 96 (5) ◽  
pp. 981-986 ◽  
Author(s):  
Nitish Sharma ◽  
Surendra Singh Rao ◽  
Namala Durga Atchuta Kumar ◽  
Annarapu Malleswara Reddy
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Intermediate Precision ◽  
Chromatography Method ◽  
Drug Products ◽  
Acquity Uplc

Abstract A selective, specific, and sensitive ultra-performance LC (UPLC) method was developed for determination of eszopiclone and its degradation products. The chromatographic separation was performed with a Waters ACQUITY UPLC system and BEH C18 column using gradient elution with mobile phases A and B. Mobile phase A was 0.01 M phosphate buffer with 0.2% (w/v) 1-octane sulfonic acid sodium salt as an ion pair reagent, adjusted pH 2.2 with orthophosphoric acid–acetonitrile (85 + 15, v/v). Mobile phase B was pH 2.2 buffer–acetonitrile (20 + 80, v/v). UV detection was performed at 303 nm. Eszopiclone and its impurities were chromatographed with a total run time of 13 min. A calibration study showed that the response for each of the impurities A, B, C, and D was linear between concentrations of 0.02 and 7.2 μg/mL (r2 ≥ 0.999). The method was validated over this range for precision, intermediate precision, accuracy, linearity, and specificity. For the precision study, RSD of each impurity was <5% (n = 6). The method was found to be precise, accurate, linear, and specific. The proposed method was successfully used for determination of eszopiclone impurities in pharmaceutical preparations.

scholarly journals Development and Validation of UPLC-ESI-MS/MS Technique for the Determination of 2-Isopropyl-4-(chloromethyl)thiazole in Ritonavir

2020 ◽  
Vol 32 (7) ◽  
pp. 1733-1740
Author(s):  
K. Durga Raja ◽  
V. Saradhi Venkata Ramana ◽  
K. Raghu Babu ◽  
B. Kishore Babu ◽  
V. Jagadeesh Kumar ◽  
...  
Keyword(s):  
High Strength ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Internal Diameter ◽  
Esi Ms ◽  
Quantitation Limit ◽  
Highly Sensitive ◽  
Liquid Chromatography Tandem Mass ◽  
Development And Validation

The objective of this work was to develop and validate a rapid, highly sensitive ultra performance liquid chromatography-tandem mass spectrometry (UPLC-ESI-MS/MS) method for the quantification of 2-isopropyl-4-(chloromethyl)thiazole in ritonavir. Chromatographic conditions of this impurity were achieved on an AQUITY UPLC column HSS (high strength silica) T3 column (100 mm long, 2.1 mm internal diameter, 1.8 μm diameter) using a gradient elution with 0.1% formic acid in water and methanol at a flow rate of 0.3 mL/min. LCMS/MS was operated under the multiple reaction mode (MRM) using electrospray ionization technique in positive ion mode and the transitions of m/z 176.1[M+H]+→140.1 for quantifier, 176.1[M+H]+→71.0 for qualifier were used to measure the impurity, respectively. The total chromatographic run time was 10 min. Full validation of the analytical method was carried out, including its system precision, selectivity, linearity, accuracy, recovery, ruggedness, stability and robustness. A linear response function was achieved in the concentration range of 0.12-1.86 μg/g with r > 0.99. The detection limit and quantitation limit of this impurity were 0.06 and 0.12 μg/g, respectively. Consistent recoveries were obtained during intra- and inter-day precision experiments in validation ranged from 80-120%. The developed method could be helpful not only for quality control and also for risk management of potential genotoxicity of this impurity in ritonavir drug substance.

scholarly journals Determination of sibutramine and phenolphthalein in weight­loss tea, coffee, and milk by ultra-­performance liquid chromatography mass spectrometry UPLC­-MS/MS

2019 ◽  
Vol 2 (4) ◽  
pp. 42-48
Author(s):  
Than Truong Van ◽  
Duy Nguyen Thanh ◽  
Kiet Ly Tuan ◽  
Vinh Hoang Ngoc ◽  
Hai Chu Van ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Formic Acid ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Distilled Water ◽  
Liquid Chromatography Mass Spectrometry ◽  
Ms Detection ◽  
Chromatography Mass Spectrometry

A rapid, simply and effective method using ultra­performance liquid chromatography coupled to mass spectrometry (MS) detection was developed in order to determine sibutramine and phenolphthalein in weight­loss tea, coffee, and milk. QuEChERS technique was used for cleaning­up sample matrices. The extracts were separated on C18 LC columns using the gradient elution of 0.1% formic acid in distilled water and acetonitrile. The recoveries at the concentration of 50 µg/kg were from 90.1 to 105.8% (with RSDR of 4.04 ­ 4.24%), from 91.9 to 100.2% (with RSDR of 3.20 ­ 4.71%), and from 86.5 to 100.5% (with RSDR of 5.17 ­ 5.49%) for weight­loss tea, coffee, and milk, respectively. Method quantitation limits were of 30 µg/kg.

scholarly journals A Validated UPLC-PDA Method for Simultaneous Determination of 3 Biologically Active Isoflavans in Trigonella stellata Extract

2020 ◽  
Vol 15 (7) ◽  
pp. 1934578X2094011
Author(s):  
Safa M. Shams Eldin ◽  
Mohamed M. Radwan ◽  
Amira S. Wanas ◽  
Abdel-Azim M. Habib ◽  
Fahima F. Kassem ◽  
...  
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Biologically Active ◽  
External Standard Method ◽  
Acid Aqueous Solution ◽  
Acquity Uplc

In this study, an ultra-performance liquid chromatography (UPLC)/photodiode array method was developed for the simultaneous determination of trigonellan glucoside (1), isotrigonellan (2), and methoxy-isotrigonellan (3) in Trigonella stellata extract using an external standard method. The extract was prepared using a standardized method by maceration of the dried plant material in ethanol. The 3 isoflavans (1-3) were separated on an Acquity UPLC C18 column using gradient elution with a mobile phase consisting of 0.1% (v/v) formic acid aqueous solution and 0.1% (v/v) formic acid in acetonitrile, and ultraviolet detection. The method provides a linear correlation for all analytes over the investigated ranges with all correlation coefficients greater than 0.998. The validated lower limits of quantitation were 53, 127, and 5 μg/mL for isoflavans 1, 2, and 3, respectively. Intraday and interday precisions (percent relative SD [RSD%]) were less than 8.3% and accuracy (RE%) ranged from 90% to 100%. The method’s capability to remain unaffected by small, but deliberate variations in method parameters (method’s reliability during normal usage) described by the robustness showed RSD% less than 4.6% measured by varying 3 different parameters. The validated method was successfully applied to simultaneously determine the concentration of the 3 new isoflavans having anti-inflammatory and antidiabetic activities. The results revealed that the validated method can be used for quality control of herbal preparations containing these or similar isoflavans that are marketed for the prevention of inflammation and as antidiabetics.

scholarly journals Simultaneous Determination of Rutin, Luteolin, Quercetin, and Betulinic Acid in the Extract ofDisporopsis pernyi(Hua) Diels by UPLC

2015 ◽  
Vol 2015 ◽  
pp. 1-5 ◽  
Author(s):  
Yanqi Wang ◽  
Shuyi Li ◽  
Dandan Han ◽  
Kehan Meng ◽  
Miao Wang ◽  
...  
Keyword(s):  
Quality Control ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Betulinic Acid ◽  
Mobile Phase ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Relative Standard ◽  
Quantitative Basis

Disporopsis pernyi(Hua) Diels, which belongs to genusDisporopsis, has been widely used for the treatment of abnormal sweating, chronic cough, and so forth. An ultra-performance liquid chromatography (UPLC) analysis was developed for the determination of rutin, luteolin, quercetin, and betulinic acid inDisporopsis pernyi(Hua) Diels roots. UPLC analysis was conducted by using a Shim-pack XR-ODS column with gradient elution with the mobile phase of acetonitrile and water containing 0.1% formic acid and with a flow rate of 0.2 mL/min, detected at 210, 254, and 280 nm. The method was precise, with relative standard deviation < 2.0%. The recoveries for the four components inDisporopsis pernyi(Hua) Diels were between 98.5 and 100.9%. The average contents of rutin, luteolin, quercetin, and betulinic acid in roots were 5.63, 2.51, 3.87, and 2.41 μg/g, respectively. The method was accurate and reproducible and it can provide a quantitative basis for quality control ofDisporopsis pernyi(Hua) Diels.

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