scholarly journals Characterization and Quantification of Phenolic Constituents in Peach Blossom by UPLC-LTQ-Orbitrap-MS and UPLC-DAD

2020 ◽  
Vol 15 (1) ◽  
pp. 1934578X1988443
Author(s):  
Yu Fu ◽  
Ruiqin Sun ◽  
Jingfan Yang ◽  
Lili Wang ◽  
Peng Zhao ◽  
...  
Keyword(s):  
Phenolic Acids ◽  
Prunus Persica ◽  
Limit Of Detection ◽  
Ultra Performance Liquid Chromatography ◽  
Array Detector ◽  
Qualitative And Quantitative Analysis ◽  
Orbitrap Mass Spectrometry ◽  
Phenolic Constituents ◽  
Limit Of Quantitation ◽  
Diagnostic Ions

Peach blossom comes from the flower of Prunus persica (L.) Batsch, which is used as herbal tea and medicine in China and Korea. It could promote defecation and alleviate the abdominal pain. In this paper, the methods, ultra-performance liquid chromatography (UPLC) method coupled with electrospray ionization hybrid linear trap quadrupole orbitrap mass spectrometry (LTQ OrbitrapMS) and UPLC system coupled with a diode array detector (DAD), were developed for the qualitative and quantitative analysis of the flavonoids and phenolic acids in peach blossoms. Eight standards were divided into 3 types according to their basic skeletons: phenolic acids, quercetin-type flavonoids, and kaempferol-type flavonoids. The MSn fragmentation behaviors and diagnostic ions of these 3 types of compounds were proposed to aid the structural identification of components in peach blossom extract. By extracting the diagnostic ions from the mass spectrum in negative mode, a total of 25 compounds, including 8 phenolic acids and 17 flavonoids, were screened out. Among these compounds, 5 compounds (chlorogenic acid, ferulic acid, rutin, hyperoside, and isoquercetrin) were quantitated by UPLC-DAD. The linearity, precision, accuracy, limit of detection, and limit of quantitation were validated for the quantification method. The validated method was applied to assay 9 batches of peach blossoms from different regions. This study was the first report on the systematic qualitative analysis of compounds in peach blossom, providing insights into the quality control of peach blossom.

Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

2021 ◽  
pp. 247263032098230
Author(s):  
Dilshad Ahmad ◽  
Faisal A. Al Meshaiti ◽  
Yazeed K. Al Anazi ◽  
Osama Al Owassil ◽  
Alaa Eldeen B. Yassin
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hybrid Nanoparticles ◽  
Array Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

scholarly journals Development and Validation of RP-HPLC Method for Quantitative Estimation of Vinpocetine in Pure and Pharmaceutical Dosage Forms

2011 ◽  
Vol 2011 ◽  
pp. 1-7 ◽  
Author(s):  
Subrata Bhadra ◽  
Sreedam Chandra Das ◽  
Sumon Roy ◽  
Shamsul Arefeen ◽  
Abu Shara Shamsur Rouf
Keyword(s):  
Limit Of Detection ◽  
Quantitative Estimation ◽  
Dosage Forms ◽  
Hplc Method ◽  
Array Detector ◽  
Acetate Solution ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Quality Control Tool

A simple, precise, specific, and accurate reversed phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for determination of vinpocetine in pure and pharmaceutical dosage forms. The different analytical performance parameters such as linearity, accuracy, specificity, precision, and sensitivity (limit of detection and limit of quantitation) were determined according to International Conference on Harmonization ICH Q2 (R1) guidelines. RP-HPLC was conducted on Zorbax C18 (150 mm length × 4.6 mm ID, 5 μm) column. The mobile phase was consisting of buffer (containing 1.54% w/v ammonium acetate solution) and acetonitrile in the ratio (40 : 60, v/v), and the flow rate was maintained at 1.0 mLmin−1. Vinpocetine was monitored using Agilent 1200 series equipped with photo diode array detector (λ = 280 nm). Linearity was observed in concentration range of 160–240 μgmL−1, and correlation coefficient was found excellent (R2 = 0.999). All the system suitability parameters were found within the range. The proposed method is rapid, cost-effective and can be used as a quality-control tool for routine quantitative analysis of vinpocetine in pure and pharmaceutical dosage forms.

scholarly journals RP-HPLC Estimation of Bumetanide and its Impurities in Oral Solid Dosage Form

2019 ◽  
Vol 31 (10) ◽  
pp. 2215-2221
Author(s):  
P. Suresh Kumar ◽  
G.V. Krishna Mohan ◽  
A. Naga Babu
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Drug Product ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Fixed Dose ◽  
Array Detector ◽  
Rp Hplc ◽  
Photodiode Array Detector ◽  
Limit Of Quantitation

A novel and simultaneous stability indicating RP-HPLC method has been developed for quantitative analysis of bumetanide in fixed dose pharmaceutical formulations. Bumetanide and its degradation products are well separated by the Discovery C18, 250 × 4.6 mm, 5 μm column as a stationary phase and (50:50 v/v) of 0.1 % o-phthalaldehyde and acetonitrile as a mobile phase. All the compounds are monitored using photodiode array detector at 254 nm with an isocratic method and the flow rate of 1.0 mL/min was maintained. Validation of method was performed as per International Council for Harmonization (ICH) guidelines and the parameters namely; precision, accuracy, specificity, stability, robustness, linearity, limit of quantitation (LOQ) and limit of detection (LOD) were evaluated. The linearity of the proposed method was found to be 0.315-1.875 μg/mL for bumetanide and its impurities. The developed method is more economical and suitable for laboratory use because of solvent consumption is very less. Hence, the developed method can be used for the determination of bumetanide and its impurities in drug product stability studies and pharmaceutical formulations.

scholarly journals Development and Validation of RP-HPLC Method for Azilsartan Medoxomil Potassium Quantitation in Human Plasma by Solid Phase Extraction Procedure

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Paras P. Vekariya ◽  
Hitendra S. Joshi
Keyword(s):  
Solid Phase Extraction ◽  
Human Plasma ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Phase Extraction ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Azilsartan Medoxomil

Simple and rapid reverse phase high-performance liquid chromatography (RP-HPLC) method was developed and validated using solid phase extraction (SPE) technique for the determination of Azilsartan Medoxomil Potassium (AMP) in human plasma; detection was carried out by photo diode array detector. Chromatographic separation of the analyte AMP was achieved within 7.5 min by Waters symmetry C18 (4.6 × 250 mm, 5 µm) column, mobile phase was 25 mM ammonium acetate buffer (pH 5.5): acetonitrile 55 : 45 v/v, flow rate was 1.0 mL/min, and the detection was carried out at 254 nm. Calibration curve was linear (r2 > 0.9985) in the range of 1.0–9.0 µg/mL, limit of detection (LOD) and limit of quantitation (LOQ) were 0.150 µg/mL and 0.400 µg/mL, respectively, and intra- and interday deviations were between 1.53–8.41% and 1.78–4.59%, respectively. The overall mean recovery of AMP was 92.35%. No any endogenous constituents were found to interfere at retention time of the analyte. This new RP-HPLC method was successfully validated and may be applied to conduct bioavailability and bioequivalence studies of AMP.

scholarly journals Effects of thermal treatments on 10 major phenolics and their antioxidant contributions in Acer truncatum leaves and flowers

2018 ◽  
Vol 5 (6) ◽  
pp. 180364 ◽  
Author(s):  
Lingguang Yang ◽  
Peipei Yin ◽  
Chi-Tang Ho ◽  
Miao Yu ◽  
Liwei Sun ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Gallic Acid ◽  
Mass Spectrometer ◽  
High Performance ◽  
Ultra Performance Liquid Chromatography ◽  
Array Detector ◽  
Diode Array ◽  
Thermal Treatments ◽  
Diode Array Detector ◽  
Phenolic Constituents

This study aimed to investigate effects of thermal treatments on major phenolics and their antioxidant contributions in Acer truncatum leaves and flowers (ATL and ATF, respectively). With ultra performance liquid chromatography-diode array detector-quadrupole time-of-flight-mass spectrometer/mass spectrometer, phenolic compositions of ATF were first characterized and compared with those of ATL. An optimized high performance liquid chromatography fingerprint was then established, and 10 major phenolics existing in both ATL and ATF were quantified. Gallic acid derivatives and flavonol-3- O -glycosides were found to be their dominant phenolic constituents, with the former being key constituents which was affected by thermal treatments and further influencing the variations of total phenols. Moreover, the mechanism underlining the changes of phenolics in ATL and ATF by the treatments was characterized as a thermolhydrolysis process. During thermal treatments, polymerized gallotannins were hydrolysed to 1,2,3,4,6-pentakis- O -galloyl-β- d -glucose, ethyl gallate and gallic acid, resulting in more than fivefold and twofold increase of their contents in ATL and ATF, respectively. By contrast, contents and antioxidant contributions of flavonol-3- O -glycosides gradually decreased during the process.\absbreak Overall, this is, to our knowledge, the first report on the effects of thermal treatments on phenolics and their antioxidant contributions in ATL and ATF, and the three gallic acid derivatives with potentially higher bioactivity could be efficiently achieved by thermal treatments.

scholarly journals Qualitative and Quantitative Analysis of the Major Constituents in Chinese Medical Preparation Lianhua-Qingwen Capsule by UPLC-DAD-QTOF-MS

2015 ◽  
Vol 2015 ◽  
pp. 1-19 ◽  
Author(s):  
Weina Jia ◽  
Chunhua Wang ◽  
Yuefei Wang ◽  
Guixiang Pan ◽  
Miaomiao Jiang ◽  
...  
Keyword(s):  
Quantitative Analysis ◽  
Limit Of Detection ◽  
Mass Measurement ◽  
Array Detector ◽  
Qualitative And Quantitative Analysis ◽  
Limit Of Quantification ◽  
Qualitative And Quantitative ◽  
Medical Preparation ◽  
Flight Mass Spectrometry ◽  
Viral Influenza

Lianhua-Qingwen capsule (LQC) is a commonly used Chinese medical preparation to treat viral influenza and especially played a very important role in the fight against severe acute respiratory syndrome (SARS) in 2002-2003 in China. In this paper, a rapid ultraperformance liquid chromatography coupled with diode-array detector and quadrupole time-of-flight mass spectrometry (UPLC-DAD-QTOF-MS) method was established for qualitative and quantitative analysis of the major constituents of LQC. A total of 61 compounds including flavonoids, phenylpropanoids, anthraquinones, triterpenoids, iridoids, and other types of compounds were unambiguously or tentatively identified by comparing the retention times and accurate mass measurement with reference compounds or literature data. Among them, twelve representative compounds were further quantified as chemical markers in quantitative analysis, including salidroside, chlorogenic acid, forsythoside E, cryptochlorogenic acid, amygdalin, sweroside, hyperin, rutin, forsythoside A, phillyrin, rhein, and glycyrrhizic acid. The UPLC-DAD method was evaluated with linearity, limit of detection (LOD), limit of quantification (LOQ), precision, stability, repeatability, and recovery tests. The results showed that the developed quantitative method was linear, sensitive, and precise for the quality control of LQC.

Simultaneous determination of ciprofloxacin hydrochloride and hydrocortisone in ear drops by high performance liquid chromatography

2014 ◽  
Vol 68 (7) ◽  
Author(s):  
Joanna Ronowicz ◽  
Bogumiła Kupcewicz ◽  
Łukasz Pałkowski ◽  
Piotr Bilski ◽  
Tomasz Siódmiak ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Array Detector ◽  
Chromatography Method ◽  
Ciprofloxacin Hydrochloride ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Ear Drops

AbstractThe aim of the study was to design and validate a reversed phase high performance liquid chromatography method for the separation and quantification of two active pharmaceutical ingredients (ciprofloxacin hydrochloride, hydrocortisone) and a preservative (benzyl alcohol) in ear drops. Effective separation of the examined compounds was achieved on a GraceSmart™ RP 18 column (150 mm × 4.6 mm, 5 μm) with gradient elution and a diode array detector. The total assay run time was 25 min. Analytical method validation assays were performed. Validation parameters used for the evaluation were: specificity, linearity, trueness, precision (repeatability and reproducibility), limit of detection and limit of quantitation. Results of the validation procedure (high recoveries, good standard deviations, no interfering peaks at the retention times corresponding to the analytes) confirm that the developed chromatographic method can be applied for routine analysis of ear drops.

scholarly journals DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE DETERMINATION OF BAMIFYLLINE HYDROCHLORIDE IN TABLET DOSAGE FORM

2017 ◽  
Vol 9 (4) ◽  
pp. 76
Author(s):  
Panchumarthy Ravisankar ◽  
Shaheem Sulthana ◽  
Inturi Mary Thanuja ◽  
A. Dihitha Chowdary ◽  
J. Vyshnavi
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Array Detector ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Photodiode Array Detector ◽  
Limit Of Quantitation ◽  
Tablet Dosage

Objective: The objective of the current study was to develop and validate a novel RP-HPLC method for determination of bamifylline hydrochloride in pharmaceutical dosage form.Methods: Chromatographic separation was conducted on Agilent technologies-1260 series with the G1311C quaternary pump, eclipse XDB C18 column (4.6 mm i.d. X 250 mm, 5 µm particle sizes) and equipped with photodiode array detector G1315D. Mobile phase consisted of methanol and acetonitrile were mixed in the ratio of 90:10 v/v, was used at a flow rate of 1 ml/min and detection wavelength was set at 263 nm.Results: The retention time for bamifylline hydrochloride was found to be 2.913 min. The calibration was linear (r2= 0.9996) in the concentration range of 2-10 µg/ml. The limit of detection and the limit of quantitation were found to be 0.4825 μg/ml and 1.4621 µg/ml respectively. Recovery of bamifylline hydrochloride in tablet formulation was observed in the range of 99.6-99.8 %. Percentage assay of bamifylline hydrochloride (Bamifix) was found to be 99.4 % w/w.Conclusion: Thus the novel proposed method for bamifylline hydrochloride was found to be feasible for the estimation of bamifylline hydrochloride in bulk as well as a pharmaceutical dosage form. 

scholarly journals A Simple Reverse Phase Ultra Performance Liquid Chromatography Validated Method for Concurrent Estimation of Daunorubicin and Cytarabine in Drug Substances and Drug Product

2020 ◽  
Vol 11 (03) ◽  
pp. 424-429
Author(s):  
Suresh Gandi ◽  
Manikandan Ayyar ◽  
Venkat Rao Sirugubattula ◽  
Murali Krishna Cheepi
Keyword(s):  
Orthophosphoric Acid ◽  
Limit Of Detection ◽  
Drug Product ◽  
Ultra Performance Liquid Chromatography ◽  
Chromatographic Technique ◽  
Reverse Phase ◽  
Drug Substances ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic ◽  
Concurrent Estimation

A fast, precise, accurate, and steadiness indicating isocratic liquid chromatographic technique was created for the synchronous assurance of the daunorubicin and cytarabine in bulk and formulation. To optimize a column CHS C18 100 × 2.1 mm, 1.8 μm, mobile phase, including buffer 0.1% orthophosphoric acid, acetonitrile pick in the proportion 70:30 v/v, was pumped through the column at a flow rate of 0.3 mL/min at 240 nm, initiate to be an efficient method for elution of drug with good peak shapes, as well as, retention times. The retention time of daunorubicin and cytarabine were initiated to be 0.556 and 0.743 minutes. The % recovery was got at 100.07 and 99.88% for daunorubicin and cytarabine separately. The limit of detection (LoD) and limit of quantitation (LoQ) values got from the relapse formula of daunorubicin and cytarabine were 0.16, 0.5, and 0.64, 1.93, correspondingly. The relapse equation of daunorubicin is y = 2974.3x + 648.32, and y = 4896.5x + 4851.5 of cytarabine.

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