scholarly journals Development of a Rapid Resolution Liquid Chromatographic Method for Simultaneous Analysis of Four Alkaloids in Rhizoma coptidis Under Different Cultivation Conditions

2009 ◽  
Vol 92 (2) ◽  
pp. 663-671 ◽  
Author(s):  
Yan-Ling Qiao ◽  
Yu-Xin Sheng ◽  
Li-Qun Wang ◽  
Jin-Lan Zhang
Keyword(s):  
Lower Limit ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Specific Method ◽  
Good Precision ◽  
Cultivation Conditions ◽  
Limit Of Quantification ◽  
Rhizoma Coptidis ◽  
Rapid Resolution

Abstract A sensitive and specific method using rapid resolution liquid chromatography coupled with UV-Vis detection was developed for fingerprint analysis of Rhizoma coptidis and simultaneous determination of 4 alkaloids: jatrorrhizine, coptisine, palmatine, and berberine. Samples of R. coptidis grown under different cultivation conditions and from different habitats were analyzed. The analysis was performed using a reversed-phase octylsilyl (C8) column and gradient elution. The mobile phase consisted of acetonitrile and 20 mmol/L KH2PO4. Each analysis was completed within 3.5 min. The method showed good linearity within test ranges of 4.7547.50 g/mL for jatrorrhizine, 20.60164.80 g/mL for coptisine, 18.07180.73 g/mL for palmatine, and 89.70717.57 g/mL for berberine. The method showed good precision, repeatability, and stability for quantification of the 4 alkaloids. The lower limit of detection was 0.19 ng for jatrorrhizine, 0.21 ng for coptisine, 0.15 ng for palmatine, and 0.14 ng for berberine. The lower limit of quantification was 0.57 ng for jatrorrhizine, 0.82 ng for coptisine, 0.55 ng for palmatine, and 0.27 ng for berberine. The overall recovery ranged from 96.30 to 104.10 for the 4 alkaloids. The method is accurate, rapid, and convenient, and it is suitable for routine quality control of R. coptidis.

Revival of physostigmine – a novel HPLC assay for simultaneous determination of physostigmine and its metabolite eseroline designed for a pharmacokinetic study of septic patients

2015 ◽  
Vol 53 (8) ◽  
Author(s):  
Nadine Pinder ◽  
Johannes B. Zimmermann ◽  
Stefan Hofer ◽  
Thorsten Brenner ◽  
Markus A. Weigand ◽  
...  
Keyword(s):  
Fluorescence Detection ◽  
Limit Of Detection ◽  
Plasma Concentrations ◽  
Internal Standard ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Pharmacokinetic Studies ◽  
Simple Liquid ◽  
Hplc Assay ◽  
Limit Of Quantification

AbstractPhysostigmine, commonly used as an antidote in anticholinergic poisoning, is reported to have additional pharmacological effects, such as activation of the cholinergic anti-inflammatory pathway in sepsis models. Due to the narrow therapeutic range of physostigmine and its metabolite eseroline, however, the plasma concentrations of these substances need to be determined so as to understand their effect and ensure safety in the treatment of septic patients.To determine physostigmine and its metabolite eseroline, a rapid and sensitive high performance liquid chromatography (HPLC) method has been developed and validated. Spiked plasma samples were cleaned up and concentrated using a simple liquid-liquid extraction (LLE) procedure with N-methylphysostigmine as internal standard. Separation was achieved using reversed-phase HPLC on a Kinetex C18 column with gradient elution and fluorescence detection (254 nm excitation/355 nm emission).LLE produced clean extracts and a mean recovery of 80.3% for eseroline and 84.9% for physostigmine. The HPLC assay revealed a limit of detection (LOD) of 0.025 ng/mL and a lower limit of quantification (LLOQ) of 0.05 ng/mL for both analytes. Linearity was observed at 0.05–10.0 ng/mL (rThe presented method is useful for human drug level monitoring of physostigmine and eseroline in accordance with current guidelines. Remarkably low plasma concentrations can be quantified after LLE with gradient elution and fluorescence detection, making this a suitable method for pharmacokinetic studies in a clinical setting.

Eco-Friendly Green Liquid Chromatographic Separations of a Novel Combination of Azelastine and Fluticasone in the Presence of their Pharmaceutical Dosage form Additives

2020 ◽  
Vol 16 (3) ◽  
pp. 277-286
Author(s):  
Amal A. El-Masry ◽  
Mohammed E. A. Hammouda ◽  
Dalia R. El-Wasseef ◽  
Saadia M. El-Ashry
Keyword(s):  
Lower Limit ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Uv Detection ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Chromatographic Separations ◽  
Pharmaceutical Dosage Form ◽  
Liquid Chromatographic

Background: The first highly sensitive, rapid and specific green microemulsion liquid chromatographic (MELC) method was established for the simultaneous estimation of fluticasone propionate (FLU) and azelastine HCl (AZL) in the presence of their pharmaceutical dosage form additives (phenylethyl alcohol (PEA) and benzalkonium chloride (BNZ)). Methods: The separation was performed on a C18 column using (o/w) microemulsion as a mobile phase which contains 0.2 M sodium dodecyl sulphate (SDS) as surfactant, 10% butanol as cosurfactant, 1% n-octanol as internal phase and 0.3% triethylamine (TEA) adjusted at pH 6 by 0.02 M phosphoric acid; with UV detection at 220 nm and programmed with flow rate of 1 mL/min. Results: The validation characteristics e.g. linearity, lower limit of quantification (LOQ), lower limit of detection (LOD), accuracy, precision, robustness and specificity were investigated. The proposed method showed linearity over the concentration range of (0.5-25 µg/mL) and (0.1-25 µg/mL) for FLU and AZL, respectively. Besides that, the method was adopted in a short chromatographic run with satisfactory resolution factors of (2.39, 3.78 and 6.74 between PEA/FLU, FLU/AZL and AZL/BNZ), respectively. The performed method was efficiently applied to pharmaceutical nasal spray with (mean recoveries ± SD) (99.80 ± 0.97) and (100.26 ± 0.96) for FLU and AZL, respectively. Conclusion: The suggested method was based on simultaneous determination of FLU and AZL in the presence of PEA and BNZ in pure form, laboratory synthetic mixture and its combined pharmaceutical dosage form using green MELC technique with UV detection. The proposed method appeared to be superior to the reported ones of being more sensitive and specific, as well as the separation was achieved with good performance in a relatively short analysis time (less than 7.5 min). Highly acceptable values of LOD and % RSD make this method superior to be used in quality control laboratories with of HPLC technique.

scholarly journals Stability-indicating HPLC-DAD assay for simultaneous quantification of hydrocortisone 21 acetate, dexamethasone, and fluocinolone acetonide in cosmetics

2020 ◽  
Vol 18 (1) ◽  
pp. 962-973
Author(s):  
Saira Arif ◽  
Sadia Ata
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Fluocinolone Acetonide ◽  
Internal Diameter ◽  
Forced Degradation ◽  
Specific Method ◽  
Regression Equations ◽  
Limit Of Quantification ◽  
Simultaneous Quantification ◽  
Relative Standard

AbstractA rapid and specific method was developed for simultaneous quantification of hydrocortisone 21 acetate (HCA), dexamethasone (DEX), and fluocinolone acetonide (FCA) in whitening cream formulations using reversed-phase high-performance liquid chromatography. The effect of the composition of the mobile phase, analysis temperature, and detection wavelength was investigated to optimize the separation of studied components. The analytes were finally well separated using ACE Excel 2, C18 AR column having 150 mm length, 3 mm internal diameter, and 2 µm particle size at 35°C using methanol with 1% formic acid and double-distilled deionized water in the ratio of 60:40 (v/v), respectively, as the mobile phase in isocratic mode. Ten microliters of sample were injected with a flow rate of 0.5 mL/min. The specificity, linearity, accuracy, precision, recovery, limit of detection (LOD), limit of quantification (LOQ), and robustness were determined to validate the method as per International Conference on Harmonization guidelines. All the analytes were simultaneously separated within 8 min, and observed retention times of HCA, DEX, and FCA were 4.5, 5.5, and 6.9 min, respectively. The proposed method showed good linearity with the correlation coefficient, R2 = 0.999 over the range of 1–150 µg/mL for all standards. The linear regression equations were y = 12.7x + 118.7 (r = 0.999) for HCA, y = 12.9x + 106.8 (r = 0.999) for DEX, and y = 12.9x + 96.8 (r = 0.999) for FCA. The LOD was 0.25, 0.20, and 0.08 µg/mL for HCA, FCA, and DEX and LOQ was 2.06, 1.83, and 1.55 µg/mL for HCA, FCA, and DEX, respectively. The recovery values of HCA, DEX, and FCA ranged from 100.7–101.3, 102.0–102.6, and 100.2–102.0%, respectively, and the relative standard deviation for precision (intra- and interday) was less than 2, which indicated repeatability and reproducibility. The novelty of the method was described by forced degradation experimentation of all analytes in the combined form under acidic, basic, oxidative, and thermal stress. The proposed method was found to be simple, rapid, and reliable for the simultaneous determination of HCA, DEX, and FCA in cosmetics.

scholarly journals Application of an LC–MS/MS Method for the Simultaneous Quantification of Homovanillic Acid and Vanillylmandelic Acid for the Diagnosis and Follow-Up of Neuroblastoma in 357 Patients

Molecules ◽  
2021 ◽  
Vol 26 (11) ◽  
pp. 3470
Author(s):  
Narae Hwang ◽  
Eunbin Chong ◽  
Hyeonju Oh ◽  
Hee Won Cho ◽  
Ji Won Lee ◽  
...  
Keyword(s):  
Lower Limit ◽  
Large Scale ◽  
Homovanillic Acid ◽  
Limit Of Detection ◽  
Method Comparison ◽  
Vanillylmandelic Acid ◽  
Limit Of Quantification ◽  
Spot Urine ◽  
Minimal Sample ◽  
Clinical Biomarkers

Homovanillic acid (HVA) and vanillylmandelic acid (VMA) are end-stage metabolites of catecholamine and are clinical biomarkers for the diagnosis of neuroblastoma. For the first time in Korea, we implemented and validated a liquid chromatography tandem mass spectrometry (LC–MS/MS) assay to measure urinary concentrations of HVA and VMA according to Clinical and Laboratory Standards Institute guidelines. Our LC–MS/MS assay with minimal sample preparation was validated for linearity, lower limit of detection (LOD), lower limit of quantification (LLOQ), precision, accuracy, extraction recovery, carryover, matrix effect, and method comparison. A total of 1209 measurements was performed to measure HVA and VMA in spot urine between October 2019 and September 2020. The relationship between the two urinary markers, HVA and VMA, was analyzed and exhibited high agreement (89.1% agreement, kappa’s k = 0.6) and a strong correlation (Pearson’s r = 0.73). To our knowledge, this is the first study to utilize LC–MS/MS for simultaneous quantitation of spot urinary HVA and VMA and analyze the clinical application of both markers on a large scale for neuroblastoma patients.

scholarly journals Surface-Enhanced Oxidation and Determination of Isothipendyl Hydrochloride at an Electrochemical Sensing Film Constructed by Multiwalled Carbon Nanotubes

2012 ◽  
Vol 2012 ◽  
pp. 1-6
Author(s):  
S. N. Prashanth ◽  
Shankara S. Kalanur ◽  
Nagappa L. Teradal ◽  
J. Seetharamappa
Keyword(s):  
Limit Of Detection ◽  
Biological Fluids ◽  
Differential Pulse ◽  
Electrochemical Sensing ◽  
Good Precision ◽  
Multiwalled Carbon ◽  
Limit Of Quantification ◽  
Surface Enhanced ◽  
Ph Range

The electrochemical behavior of isothipendyl hydrochloride (IPH) was investigated at bare and multiwalled-carbon-nanotube modified glassy carbon electrode (MWCNT-GCE). IPH (55 μM) showed two oxidation peaks in Britton-Robinson (BR) buffer of pH 7.0. The oxidation process of IPH was observed to be irreversible over the pH range of 2.5–9.0. The influence of pH, scan rate, and concentration of the drug on anodic peak was studied. A differential pulse voltammetric method with good precision and accuracy was developed for the determination of IPH in pure and biological fluids. The peak current was found to be linearly dependent on the concentration of IPH in the range of 1.25–55 μM. The values of limit of detection and limit of quantification were noticed to be 0.284 and 0.949 μM, respectively.

DEVELOPMENT OF VALIDATED RP-HPLC METHOD FOR THE QUANTITATIVE ANALYSIS OF CHROMIUM PICOLINATE III IN A DIET VINEGAR FORMULATION

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (05) ◽  
pp. 48-52
Author(s):  
A Lodhi ◽  
◽  
A Jain ◽  
B. Biswal
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Chromium Picolinate ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A validated high performance liquid chromatographic method was developed for the determination of chromium picolinate in pharmaceutical dosage forms. The analysis was performed at room temperature using a reversed-phase ODS, 5µm (250×4.6) mm column. The mobile phase consisted of acetonitrile: buffer (60:40 V/V) at a flow rate of 0.5 mL/min. The PDA-detector was set at 264 nm. The developed method showed a good linear relationship in the concentration range from 1.5 – 12.5 µg/mL with a correlation coefficient from 0.999. The limit of detection and limit of quantification were 0.0540513 and 0.1637919 µg/mL respectively.

Determination of tigecycline in turkey plasma by LC-MS/MS: validation and application in a pharmacokinetic study

2017 ◽  
Vol 20 (2) ◽  
pp. 241-249 ◽  
Author(s):  
A. Jasiecka-Mikołajczyk ◽  
J.J. Jaroszewski
Keyword(s):  
Pharmacokinetic Study ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Reversed Phase ◽  
Selected Reaction Monitoring ◽  
Limit Of Quantification ◽  
Complicated Skin ◽  
Intravenous And Oral Administration

Abstract Tigecycline (TIG), a novel glycylcycline antibiotic, plays an important role in the management of complicated skin and intra-abdominal infections. The available data lack any description of a method for determination of TIG in avian plasma. In our study, a selective, accurate and reversed-phase high performance liquid chromatography-tandem mass spectrometry method was developed for the determination of TIG in turkey plasma. Sample preparation was based on protein precipitation and liquid-liquid extraction using 1,2-dichloroethane. Chromatographic separation of TIG and minocycline (internal standard, IS) was achieved on an Atlantis T3 column (150 mm × 3.0 mm, 3.0 μm) using gradient elution. The selected reaction monitoring transitions were performed at 293.60 m/z → 257.10 m/z for TIG and 458.00 m/z → 441.20 m/z for IS. The developed method was validated in terms of specificity, selectivity, linearity, lowest limit of quantification, limit of detection, precision, accuracy, matrix effect, carry-over effect, extraction recovery and stability. All parameters of the method submitted to validation met the acceptance criteria. The assay was linear over the concentration range of 0.01-100 μg/ml. This validated method was successfully applied to a TIG pharmacokinetic study in turkey after intravenous and oral administration at a dose of 10 mg/kg at various time-points.

scholarly journals ESTIMATION OF GUGGULSTERONE-Z IN GOKSHURADI GUGGULU USING REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2018 ◽  
Vol 11 (11) ◽  
pp. 204
Author(s):  
Kanan G Gamit ◽  
Niraj Y Vyas ◽  
Nishit D Patel ◽  
Manan A Raval
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Photodiode Array Detector ◽  
Validation Parameters ◽  
Photodiode Array

Objective: A study was aimed to estimate guggulsterone-Z (GZ) in Gokshuradi Guggulu (GG).Methods: An analytical method was developed and validated using Waters Alliance high-performance liquid chromatography system (Empower software), equipped with photodiode array detector. Separation was achieved using Phenomenex, C-18 (250 mm×4.6 mm, 5 μ) column. Mobile phase consisted of acetonitrile:water (70:30,v/v). Flow rate was set to 1 ml/min and detection was performed at 251 nm.Results and Discussion: Validation parameters such as linearity, precision, accuracy, limit of detection, limit of quantification, and robustness were performed. Amount of GZ was estimated using linearity equation.Conclusion: GG was found to contain 0.815±0.03 g% w/w GZ. Validated method may be used as one of the parameters to standardize the formulation.

scholarly journals METHOD DEVELOPMENT AND VALIDATION OF LOPINAVIR IN TABLET DOSAGE FORM USING REVERSED-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2018 ◽  
Vol 11 ◽  
Author(s):  
Sunkara Namratha ◽  
Vijayalakshmi A
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Liquid Chromatographic

Objective: Reversed-phase high-performance liquid chromatographic method (RP-HPLC) was developed for the assessment of lopinavir in the dosage form of tablet.Methods: Chromatogram was run through using Kromosil C18 4.5×150 mm using a mobile phase methanol: water of ratio 65:35% v/v with a rate of flow of 0.8 ml/min, measured by UV spectrometric detection at 265 nm. The method developed was validated in terms of precision, accuracy, linearity, and robustness parameters.Results: Retention time of lopinavir established at 2.482 min and percentage R.S.D of lopinavir found to be 1.0% and 0.5%, respectively. The method shows that good linearity range of 30–150 μg correlation coefficient of lopinavir was 0.997. The limit of detection was 2.97 and limit of quantification was 9.92, respectively. The percent purity of lopinavir was 99.87%.Conclusion: The suggested method (Rp-HPLC) for concurrent assay lopinavir was validated, which is appropriate method for the analysis oflopinavir quantitatively in tablet dosage forms and bulk.

Chlorobenzene. Determination in workplace air

2019 ◽  
Vol 35 (1(99)) ◽  
pp. 19-28
Author(s):  
Anna Jeżewska ◽  
Agnieszka Woźnica
Keyword(s):  
Occupational Exposure ◽  
Carbon Disulfide ◽  
Limit Of Detection ◽  
Skin Irritation ◽  
Raw Material ◽  
Good Precision ◽  
Limit Of Quantification ◽  
Selective Determination ◽  
Workplace Air

Chlorobenzene is a colorless, flammable liquid that has an almond-like odor. It is used in industry as a solvent: resins, paints and fats, raw material for the production of plastics, as well as for the production of phenol, aniline and nitrobenzene. Occupational exposure to chlorobenzene vapors can occur through inhalation, absorption through the skin or ingestion. Harmful if inhaled, causes skin irritation. Long-term exposure affects the central nervous system. The aim of this study was an amendment to the PN-Z-04022- 03:2001 withdrawn from the Polish set of standards, and validate method for determination concentrations of chlorobenzene in the workplace air in the range from 1/10 to 2 MAC values, in accordance with the requirements of the standard PN-EN 482. The study was performed using a gas chromatograph (GC) with a flame ionization detector (FID) equipped with a capillary column HP-5 (30 m x 0.32 mm, 0.25 μm). This method is based on the adsorption of chlorobenzene vapors on activated charcoal, desorption with carbon disulfide, and analyzed by GC-FID. Application of HP-5 column allows selective determination of chlorobenzene in a presence of carbon disulfide, aniline, phenol and nitrobenzene. The measurement range was 2.3 ÷ 46 mg/m3 for a 15 l air sample. Limit of detection: 6.75 ng/ml and limit of quantification: 20.25 ng/ml. Analytical method described in this paper enables selective determination of chlorobenzene in workplace atmosphere in presence of other solvents at concentrations from 2.3 mg/m3 (1/10 MAC value). The method is characterized by good precision and accuracy and meets the criteria for the performance of procedures for the measurement of chemical agents, listed in EN 482. The method may be used for the assessment of occupational exposure to chlorobenzene and the associated risk to workers’ health. The developed method of determining chlorobenzene has been recorded as an analytical procedure (see Appendix). This article discusses the problems of occupational safety and health, which are covered by health sciences and environmental engineering.

Sign in / Sign up

Export Citation Format

Share Document