Multi-Index Quantitative Evaluation of Angelicae sinesis Radix Based on 1H-qNMR

2020 ◽  
Vol 103 (6) ◽  
pp. 1633-1638
Author(s):  
Yu Zhang ◽  
Qian Li ◽  
Yanmei Feng ◽  
Lan Yang ◽  
Daiyu Qiu ◽  
...  
Keyword(s):  
Ferulic Acid ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Accurate Method ◽  
Scientific Basis ◽  
Hplc Method ◽  
Active Components ◽  
Limit Of Quantification ◽  
Significant Difference ◽  
Angelicae Sinensis

Abstract Background As known to us, HPLC method was often used to determine the contents of Angelicae sinesis Radix. In view of the shortcomings of HPLC method, qNMR has prominent advantages in determining the contents of bioactive components in the quantitative and qualitative analysis of Angelicae sinesis Radix. Objective In this study, a quick, simple, and accurate method was established to determine the components of ferulic acid, coniferyl ferulate, and ligustilide in Angelicae sinesis Radix. Method Using dimethyl sulfoxide-d6(DMSO-d6) as the test solvent and pyrazine as the internal standard substance, 1H-qNMR measurement was performed on a 600 MHz spectrometer. The quantitative resonance peaks of pyrazine, ferulic acid, ligustilide, and coniferyl ferulate were at δ8.66 ppm, δ6.35–6.37 ppm, δ5.53–5.55 ppm, and δ6.50–6.53 ppm, respectively. Results The linear relationship, limit of detection, limit of quantification, precision, stability, and recovery were verified and the results were good. On the other hand, it was verified by HPLC, and the HPLC used for verification passed the methodological investigation of linearity, precision, repeatability, stability, and recovery, and the results were good. In addition, no significant difference in results was found between the 1H-qNMR and HPLC-UV methods in determining the content of three components in three batches of Angelicae sinesis Radix. Conclusions The method can be used for simultaneous determination of three active components, and providing a scientific basis for the overall quality evaluation and quality control of Angelicae sinesis Radix. Hightlights In this study, 1H-qNMR was used to determine ferulic acid, coniferyl ferulate and ligustilide in Angelicae Sinensis Radix for the first time.

scholarly journals Simultaneous Determination of Eight Chemical Components in Angelicae Sinensis Radix and Its Herbal Products by QAMS

2021 ◽  
Vol 2021 ◽  
pp. 1-7
Author(s):  
Yu Zhang ◽  
Qian Li ◽  
Yanmei Feng ◽  
Lan Yang ◽  
Qi Wang ◽  
...  
Keyword(s):  
Quantitative Analysis ◽  
Ferulic Acid ◽  
Internal Standard ◽  
Chemical Components ◽  
Herbal Products ◽  
Standard Substance ◽  
External Standard Method ◽  
Significant Difference ◽  
Single Marker ◽  
Angelicae Sinensis

A HPLC method has been developed for simultaneously detecting chlorogenic acid, ferulic acid, senkyunolide I, senkyunolide H, coniferyl ferulate, senkyunolide A, ligustilide, and levistolide A in Angelicae Sinensis Radix through quantitative analysis of multicomponents by single-marker (QAMS) method with ferulic acid as internal standard substance. The relative analysis correction factors of each component in Angelicae Sinensis Radix have good reproducibility under different chromatography conditions. In addition, no significant difference of results was found between quantitative analysis of multicomponents by single-marker (QAMS) method and external standard method in determining content of these components of different Angelicae Sinensis Radix and its 12 kinds of preparations. As a result, the established QAMS method for Angelicae Sinensis Radix analysis with ferulic acid as internal standard substance is accurate and feasible, which could be used as an effective and economical method to control quality of Angelicae Sinensis Radix and its herbal products.

scholarly journals Development and Validation of an HPLC Method for the Analysis of Chlorpropham and 3-Chloroaniline in Potato Extracts

2014 ◽  
Vol 2014 ◽  
pp. 1-5 ◽  
Author(s):  
Nidhal M. Sher Mohammed ◽  
T. H. Flowers ◽  
H. J. Duncan
Keyword(s):  
Limit Of Detection ◽  
Internal Standard ◽  
Potato Industry ◽  
Hplc Method ◽  
Coefficient Of Determination ◽  
Repeated Injection ◽  
Good Separation ◽  
Limit Of Quantification ◽  
Development And Validation ◽  
Good Agreement

Chlorpropham (CIPC) is the main sprout inhibitor used by potato industry. There is concern about the residues of CIPC and its degradation product 3-chloroaniline, 3-CA; hence, analytical methods are required to analyse their residues in potato samples. An HPLC-UV method was developed and validated for the separation and quantification of these compounds using propham (IPC) as an internal standard. The chromatographic conditions required to achieve good separation were 60% mobile phase of methanol, 15-minute run time at a flow rate of 1.5 mL/min, and a detection wavelength of 210 nm using Phenomenex (ODS-2 250 mm × 4.60 mm 5 µm Sphereclone) column at an ambient temperature. The method was validated for precision, linearity, the limit of detection (LOD) and the limit of quantification (LOQ), producing high precision through RSD ≤ 0.03%, and acceptable criteria of the coefficient of determination (R2) of the calibration curves (0.990). LOD values of CIPC and 3-CA were approximately 0.01 µg/mL whereas the LOQ values were approximately 0.04 µg/mL using repeated injection approach. The proposed HPLC method was compared with the standard GC method of the CIPC residues extracted showing good agreement R2=0.99. Despite using the same extract, the recovery results for the proposed HPLC method were 13% higher than GC analysis.

Pharmacokinetic Study of Main Active Components of Rumex nepalensis Spreng Extract in Rats Plasma by UPLC-MS/MS

2019 ◽  
Vol 15 (4) ◽  
pp. 371-378
Author(s):  
Jin Wang ◽  
Yang Chu ◽  
Xiao Li ◽  
Navaneethakrishnan Polachi ◽  
Xue-ying Yan ◽  
...  
Keyword(s):  
Pharmacokinetic Study ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Tandem Mass ◽  
Active Components ◽  
Limit Of Quantification ◽  
Liquid Chromatography Tandem Mass ◽  
Acquity Uplc

Background: The Rumex nepalensis Spreng (RNS) is a traditional Chinese medicine containing rich anthraquinones. However, through proper investigation we have found that there were no reports on the pharmacokinetics of RNS extract in rats. </P><P> Objective: We study on the pharmacokinetic behaviors of emodin, chrysophanol and physcion after oral administration of RNS extract in rat to achieve a better understanding of further clinical application and conduct the preparation development of the herb. Methods: In the present study, a sensitive and rapid ultra-fast liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed and validated to determine the three anthraquinones such as chrysophanol, emodin and physcion in rat plasma along with danthron as the internal standard (IS). The analytes and IS were separated on an Acquity UPLC HSS T3 column (100 mm × 2.1 mm, 1.8 µm) by using the mobile phase of water with 3 mM ammonium acetate and acetonitrile as gradient elution at a flow rate of 0.4 mL min -1. The detection was performed on a triple quadrupole tandem mass spectrometer equipped with electrospray ionization (ESI) by multiple reactions monitoring (MRM) of the transitions at m/z 253.1 → 225.0 for chrysophanol, 269.0 → 224.9 for emodin, 282.7→ 240.0 for physcion and m/z 239.0 → 211.0 for IS. The limit of detection and lower limit of quantification were both 2 ng mL -1 in rat plasma. Results: Good linearity of this method was obtained in the range of 2-1000 ng mL -1 , and the correlation coefficient was greater than 0.990. According to regulatory guidelines, the established method was fully validated, and the results were within acceptable limits. Conclusion: The validated method was successfully applied into a pharmacokinetic study of orally administered RNS extract in rats.

scholarly journals DEVELOPMENT AND VALIDATION OF CARBAMAZEPINE PLASMA CONCENTRATIONS MEASUREMENT AND ITS APPLICATION ON EPILEPSY PATIENTS

2017 ◽  
Vol 9 (9) ◽  
pp. 87 ◽  
Author(s):  
Astri Budikayanti ◽  
Chiswyta Chaliana ◽  
Melva Louisa ◽  
Rianto Setiabudy
Keyword(s):  
Lower Limit ◽  
High Performance ◽  
Limit Of Detection ◽  
Plasma Concentrations ◽  
Internal Standard ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Precision And Accuracy ◽  
Development And Validation

Objective: To develop and validate high-performance liquid chromatography with photodiode array (HPLC-PDA) detector as a method for measuring carbamazepine plasma concentrations in epilepsy patients treated with monotherapy or polytherapy.Methods: Carbamazepine was extracted from epilepsy patients’ plasma through liquid-liquid extraction, using protein precipitation with chloroform. Analysis was performed using HPLC with Inertsil DS-4 C18 (4.6x150 mm), 5 μm particle size column. The optimal condition for separation was established in a mobile phase consisting of acetonitrile: water (50:50) at a flow rate of 1.0 ml/min, detected by PDA detector at 220 nm. Propylparaben was used as the internal standard. The retention time was 3.5 min.Results: Linearity was obtained over a concentration range of 0.5-16 μg/ml with r = 0.999. The method showed good intra-and inter-day precision and accuracy of more than 90% difference (% diff) and 95% relative standard deviation (RSD). Lower limit of quantification (LOQ) was 0.5 μg/ml and lower limit of detection (LOD) was 0.2 μg/ml with 100% accuracy and more than 90% precision. Recovery test was nearly 100%. Stability of carbamazepine plasma concentration in 3 epilepsy patients was measured on the first and third month of treatment, ranging between 83.5 to 98.7%. When used to compare carbamazepine as a monotherapy versus polytherapy, the method showed good selectivity.Conclusion: The present HPLC method was valid for measuring carbamazepine plasma concentrations in epilepsy patients treated with monotherapy or polytherapy. This method meets the standard in the EMEA guideline in terms of linearity, precision, and accuracy, also selectivity in epilepsy patients treated with polytherapy.

DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR AMISULPRIDE IN BULK AND PHARMACEUTICAL FORMULATION

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (04) ◽  
pp. 43-50
Author(s):  
K. M. L Manoja ◽  
◽  
B. M. Gurupadayya ◽  
S Srujana ◽  
L. V. Raaga ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Forced Degradation ◽  
Uv Detector ◽  
Limit Of Quantification

A simple, sensitive, rapid, robust and reproducible method for the determination of amisulpride using paracetamol as internal standard (IS) in bulk and pharmaceutical formulation was developed using reverse phase high performance liquid chromatographic method. The analysis was performed on C18 (250 4.6 mm, 5 mcm) column with a mobile phase consisting of 0.03 M potassium dihydrogen ortho phosphate buffer (pH 6.5), acetonitrile in the ratio of 67:33 (V/V) with a flow rate of 1 mL/min. The analyte was monitored with UV detector at 263 nm. In the developed method amisulpride elutes at retention time of 4.4 min and paracetamol (IS) at 3.3 min. The proposed method is having linearity in the concentration range from 10-100 mcg/mL of amisulpride. The method was validated with respect to system suitability, linearity, precision, limit of detection (LOD) and limit of quantification (LOQ), accuracy (recovery),ruggedness, robustness, stability, forced degradation studies (specificity). The proposed method can be readily utilized for bulk drug and pharmaceutical formulations of amisulpride.

scholarly journals Validated RP-HPLC Method for the Assay of Etoricoxib (A Non-Steroidal Anti-Inflammatory Drug) in Pharmaceutical Dosage Forms

2012 ◽  
Vol 9 (2) ◽  
pp. 832-838 ◽  
Author(s):  
Srinivasu Topalli ◽  
T. G. Chandrashekhar ◽  
M. Mathrusri Annapurna
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms

A simple, accurate, sensitive and reproducible reverse phase high performance liquid chromatographic method has been developed for the quantitative determination of Etoricoxib in pharmaceutical dosage forms. The assay was performed on Hypersil ODS C-18 (250 x 4.6 mm., 5µm particle size) column using acetonitrile and potassium dihydrogen phosphate buffer (pH 4.2) (46:54 % v/v) as mobile phase with UV detection at 280 nm (flow rate 1.2 ml/min). Bromhexine was used as an internal standard. Quantization was achieved by measurement of the peak area ratio of the drug to the internal standard. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.0704 µg ml-1and 0.2134 µg ml-1respectively. Each analysis required no longer than 10 minutes. The calibration curve was linear over the concentration range from 0.5-85.0 µg ml-1. The retention times of Etoricoxib and Bromhexine were found to be 3.083 and 7.631 minutes respectively. The proposed method was validated according to the ICH guidelines and can be used successfully to analyse marketed formulations.

scholarly journals Development and validation of a simple and rapid UPLC method for the in-vitro estimation of (-)-epigallocatechin-3-gallate in lipid-based formulations

2018 ◽  
Vol 9 (1) ◽  
pp. 7-12 ◽  
Author(s):  
Maha Osama El-Kayal ◽  
Maha Nasr Sayed ◽  
Nahed Dawood Mortada ◽  
Seham Elkheshen
Keyword(s):  
Analytical Method ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Potential Health ◽  
Validation Parameters ◽  
Significant Difference ◽  
Lipid Based Formulation

(-)-Epigallocatechin gallate (EGCG) is a catechin found in green tea that has potential health benefits, such as anti-oxidant, anti-carcinogenic and anti-inflammatory effects. A rapid and sensitive Ultra-Performance Liquid Chromatographic (UPLC) method was developed and validated for the estimation of (-)-epigallocatechin-3-gallate in lipid-based formulation. The UPLC method was conducted on C18 analytical column (50 mm × 2.1 mm, 1.8 μm particle size). The mobile phase consisted of a mixture of acetic acid (1%, v:v; pH = 3), acetonitrile and water at volume ratio of 13:15:72 delivered at a flow rate of 0.5 mL/min. The diode array detector (DAD) acquisition wavelength was set at wavelengths 210 and 280 nm. Caffeine was used as internal standard. The tested validation parameters, i.e., selectivity, linearity, accuracy, precision, and sensitivity (Limit of detection and limit of quantification) were determined at both wavelengths. Results revealed that caffeine and EGCG peaks were eluted at retention times of 0.55 and 0.85 minutes, respectively. The calibration curve was linear over the concentration range of 10-60 μg/mL, with coefficients of determination (r2) of 0.9993 and 0.9998 nm at 210 and 280 nm, respectively. All the validation parameters were found within the acceptable range. The proposed method was successfully applied for the quantitation of EGCG in lipid-based formulation and statistical analysis with a reported method showed no significant difference at p < 0.05. Therefore, the proposed analytical method for EGCG can be considered as a rapid, selective and accurate analytical method that can be used for the quantitative analysis of EGCG.

scholarly journals A NOVEL, SIMPLE, RAPID RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF FERULIC ACID, QUERCETIN, PIPERINE AND THYMOL IN AYURVEDIC FORMULATION

2018 ◽  
Vol 10 (6) ◽  
pp. 303
Author(s):  
Vandana Jain ◽  
Shaikh Heena
Keyword(s):  
Ferulic Acid ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Potassium Dihydrogen ◽  
Rp Hplc ◽  
Quantification Accuracy ◽  
The Mean

Objective: A simple, accurate, precise and robust reverse phase high performance liquid chromatography (RP-HPLC) method was developed for simultaneous estimation of ferulic acid, quercetin, piperine and thymol in marketed ayurvedic formulation.Methods: The selected markers were resolved using shim pack GIST C-18 column, with mobile phase acetonitrile: 0.04 M potassium dihydrogen ortho phosphate buffer (pH 3.0 adjusted with ortho phosphoric acid) in a ratio of 60:40 v/v at a flow rate of 1.0 ml/min. The detection was carried out at 264 nm.Results: The retention time of ferulic acid, quercetin, piperine and thymol were found to be 2.98, 3.35, 7.83 and 9.72 min respectively. The developed method was validated according to the guidelines provided in ICH Q2 (R1) in term of linearity, precision, limit of detection, limit of quantification, accuracy and robustness. Linear response for all selected markers was obtained in the concentration range of 12-28 µg/ml with a correlation coefficient (r2) greater than 0.999. The mean % recovery was found to be 99.30 for ferulic acid, 98.77 for quercetin, 100.93 for piperine and 100.25 for thymol.Conclusion: The developed method was applied for quantification of these marker in marketed ayurvedic formulation. This method can be used to evaluate other formulations containing these selected phytoconstituent, thus conforming the quality and safety of ayurvedic or polyherbal formulations.

scholarly journals RP-HPLC Method for the Estimation of Nebivolol in Tablet Dosage Form

2009 ◽  
Vol 6 (3) ◽  
pp. 915-919 ◽  
Author(s):  
M. K. Sahoo ◽  
R. K. Giri ◽  
C. S. Barik ◽  
S. K. Kanungo ◽  
B. V. V. Ravi Kumar
Keyword(s):  
Dosage Form ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Accuracy And Precision ◽  
Tablet Dosage

A reverse phase HPLC method is described for the determination of nebivolol in tablet dosage form. Chromatography was carried on a Hypersil ODS C18column using a mixture of methanol and water (80:20 v/v) as the mobile phase at a flow rate of 1.0 mL/min with detection at 282 nm. Chlorzoxazone was used as the internal standard. The retention times were 3.175 min and 4.158 min for nebivolol and chlorzoxazone respectively. The detector response was linear in the concentration of 1-400 μg/mL. The limit of detection and limit of quantification was 0.0779 and 0.2361 μg/mL respectively. The percentage assay of nebivolol was 99.974%. The method was validated by determining its sensitivity, accuracy and precision. The proposed method is simple, fast, accurate and precise and hence can be applied for routine quality control of nebivolol in bulk and tablet dosage form.

scholarly journals Development and Validation of a HPLC Method to Determine Griseofulvin in Rat Plasma: Application to Pharmacokinetic Studies

2008 ◽  
Vol 3 ◽  
pp. ACI.S953 ◽  
Author(s):  
Bo Wei ◽  
Dong Liang ◽  
Theodore R. Bates
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Rat Plasma ◽  
Hplc Method ◽  
Pharmacokinetic Studies ◽  
Dihydrogen Phosphate ◽  
Sodium Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Sodium Dihydrogen

A simple, specific, sensitive, and rapid high performance liquid chromatography (HPLC) method for the determination of griseofulvin in small volumes of rat plasma was developed and validated using warfarin as an internal standard. Biological sample preparation involved simple extraction with acetonitrile, followed by dilution with aqueous mobile phase buffer (20 mM sodium dihydrogen phosphate, pH 3.5) to eliminate any chromatographic solvent effects. Griseofulvin and warfarin were baseline separated and quantitated on a C18 reversed phase column (4.6 x 150 mm, 3.5 µm), using a mobile phase composed of a 20 mM aqueous solution of sodium dihydrogen phosphate-acetonitrile (55:45, v/v, pH 3.5) delivered at a flow rate of 1.0 mL/min, and with fluorescence detection (λexcitation = 300 nm, λemission = 418 nm). The method was proven to be linear over a plasma griseofulvin concentration range of 10 to 2500 ng/mL with a mean correlation coefficient of 0.9996. The intra-day and inter-day accuracy (relative error) were in the range of 0.89% to 9.26% and 0.71% to 7.68%, respectively. The within-day precision (coefficient of variation) was less than 3.0% and the between-day precision was less than 7.5%. The mean recovery of griseofulvin from rat plasma was found to be 99.2%. The limit of detection (LOD) and the limit of quantification (LOQ) of griseofulvin were determined to be 1 ng/mL and 10 ng/mL, respectively. The developed method was successfully applied to quantitatively assess the pharmacokinetics of griseofulvin in rats following a single 50 mg/kg oral dose of the drug.

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