scholarly journals Simultaneous Determination of 13 Chemical Marker Compounds in Gwakhyangjeonggi-san, a Herbal Formula, with Validated Analytical Methods

2014 ◽  
Vol 9 (1) ◽  
pp. 1934578X1400900
Author(s):  
Jung-Hoon Kim ◽  
Hyeun-Kyoo Shin ◽  
Chang-Seob Seo

This study was designed for simultaneous determination of 13 chemical marker compounds, namely, protocatechuic acid, chlorogenic acid, caffeic acid, liquiritin, hesperidin, apigetrin, rosmarinic acid, oxypeucedanin hydrate, byakangelicin, apigenin, glycyrrhizin, nobiletin, and 6-gingerol in Gwakhyangjeonggi-san (GJS: Huoxiang-zhengqi-san in Chinese). A quantitative analytical method was developed based on HPLC-PDA with validation in terms of precision, accuracy, and repeatability, and successfully employed for quality evaluation of GJS samples with the help of chemometric techniques such as principal component analysis (PCA) and hierarchical clustering analysis (HCA). The correlation coefficient for the linear regression was > 0.9994. The intra-day and inter-day precision was < 3.0% of the relative standard deviation (RSD) value, and the recovery was in the range 92.5–107.0%, with RSD values < 4.0%, and the repeatability was < 3.0% of RSD. Variations in the quantity were observed in GJS products from different origins, which were classified by PCA and HCA. The quantitative and chemometric analyses indicate the necessity for consistency in GJS production for the purpose of quality control.

2020 ◽  
Vol 10 (16) ◽  
pp. 5482
Author(s):  
Beom-Geun Jo ◽  
Kyung-Hwa Kang ◽  
Min Hye Yang

Haedoksamul-tang (HST) is a traditional medical prescription comprising eight medicinal herbs: Angelica gigas, Cnidium officinale, Coptis japonica, Gardenia jasminoides, Paeonia lactiflora, Phellodendron amurense, Rehmannia glutinosa, and Scutellaria baicalensis. HST is used to treat blood circulation disorders and has anti-inflammatory, hemostatic, and anticonvulsant effects. In this study, a high-performance liquid chromatography/photodiode array detector (HPLC–PDA) method was developed and validated for the simultaneous determination of four marker compounds in HST, namely, berberine, palmatine, geniposide, and paeoniflorin. Four standard solutions and HST sample solutions were analyzed using a reverse-phase SunFire®C18 column (4.6 × 250 mm, 5 μm) using a 0.05% aqueous formic acid/methanol gradient. The column temperature, flow rate, injection volume, and wavelengths used were 28 ± 2 ℃, 1.0 mL/min, 10.0 μL, and 230 nm and 240 nm, respectively. Calibration curves of the four marker compounds showed good linearity (r2 ≥ 0.9994), and limits of detection (LODs) and quantification (LOQs) were in the ranges 0.131–0.296 μg/mL and 0.398–0.898 μg/mL, respectively. Ranges of intra- and inter-day precisions and accuracies values were 96.74–102.53% and 97.95–100.83%, respectively, and relative standard deviation (RSD) values were all <4%. Recoveries averaged 92.33–116.72% with RSD values <5%. Quantitative analysis for the four marker compounds showed geniposide (10.77 mg/g) was most abundant in HST.


2019 ◽  
Vol 15 (5) ◽  
pp. 542-553
Author(s):  
Hui Zhao ◽  
Hao Cai ◽  
Juan-Xiu Liu ◽  
Sheng-Nan Wang ◽  
Xun-Hong Liu ◽  
...  

Background: Xanthium sibiricum is a well-known traditional Chinese medicine (TCM) that has been commonly used to treat rhinitis and related nasal diseases. The aim of this study was to develop a comprehensive analytical method based on high-performance liquid chromatographyelectrospray ionization coupled with triple quadrupole-linear ion trap mass spectrometry (LC-ESIQTRAP- MS/MS) for the simultaneous determination of phenolic acids, anthraquinones, and flavonoids in the aerial part and fruit of Xanthium sibiricum. Methods: The separation was completed on Agilent ZORBAX SB-C18 column (250 × 4.6 mm, 5μm) using methanol and 0.2% (v/v) aqueous formic acid as the mobile phase. The target components were analyzed in negative ion mode with accurate and sensitive multiple reaction monitoring (MRM) mode. Results: The correlation coefficients of all the calibration curves were higher than 0.9994. Relative standard deviations of intra- and inter-day precisions of the eighteen components were all lower than 2.87% and the recoveries were in the range from 97.73% to 101.82%. The validated method was successfully applied to possess forty Xanthium sibiricum samples (Xanthii Herba, Xanthii Fructus, and processed Xanthii Fructus) collected from different places in P. R. China. Furthermore, principal component analysis (PCA) was performed to evaluate and classify the samples according to the contents of the eighteen bioactive components. Conclusion: All the results demonstrated that the developed method was useful and could be applied for the overall assessment of the quality of Xanthii Herba and Xanthii Fructus.


PeerJ ◽  
2020 ◽  
Vol 8 ◽  
pp. e9083
Author(s):  
Yuan Chen ◽  
Yanyun Hong ◽  
Daofu Yang ◽  
Zhigang He ◽  
Xiaozi Lin ◽  
...  

Background As the major bioactive compounds in citrus and grape, it is significant to use the contents of flavonoids and phenolic acids as quality evaluation criteria to provide a better view of classifying the quality and understanding the potential health benefits of each fruit variety. Methods A total of 15 varieties of citrus and 12 varieties of grapes were collected from Fujian, China. High-performance liquid chromatography method was used for the simultaneous determination of 17 phenolic compounds, including gallic acid, chlorogenic acid, caffeic acid, syringic acid, ρ-coumaric acid, ferulic acid, benzoic acid, salicylic acid, catechin, epicatechin, resveratrol, rutin, naringin, hesperidin, quercetin, nobiletin and tangeritin in the peels of citrus and grape cultivars. Further, the cultivars of citrus and grape were classified using principal component analysis (PCA) and hierarchical cluster analysis (HCA). Results A thorough separation of the 17 compounds was achieved within 100 min. The tested method exhibited good linearity (the limits of detection and limits of quantification were in the range of 0.03–1.83 µg/mL and 0.09–5.55 µg/mL, respectively), precision (the relative standard deviations of repeatability were 1.02–1.97%), and recovery (92.2–102.82%) for all the compounds, which could be used for the simultaneous determination of phenolic compounds in citrus and grape. Hesperidin (12.93–26,160.98 µg/g DW) and salicylic acid (5.35–751.02 µg/g DW) were the main flavonoids and phenolic acids in 15 citrus varieties, respectively. Besides, the hesperidin (ND to 605.48 µg/g DW) and salicylic acid (ND to 1,461.79 µg/g DW) were found as the highest flavonoid and the most abundant phenolic acid in grapes, respectively. A total of 15 citrus and 12 grape samples were classified into two main groups by PCA and HCA with strong consistency.


2016 ◽  
Vol 11 (11) ◽  
pp. 1934578X1601101 ◽  
Author(s):  
Chang-Seob Seo ◽  
Hyeun-Kyoo Shin

In Korean folk medicine, Melandrium firmum Rohrbach (Caryophyllaceae) has been used to treat various diseases, including anuria, breast cancer, and gonorrhea. In this study, a high-performance liquid chromatography method with photodiode-array UV detection (HPLC-PDA) was established and then validated for the simultaneous determination of five flavonoids in M. firmum: schaftoside, homoorientin, cytisoside, vitexin, and isovitexin. Separation of the five compounds was performed on a Gemini C18 column at 40°C by gradient elution of two mobile phases. The flow rate and injection volume were 1.0 mL/min and 10 μL, respectively. The HPLC-PDA method showed excellent linear regression with r2 values of 0.9999 within the test ranges. The limits of detection and quantification of all components were 0.01–0.11 and 0.04–0.34 μg/mL, respectively. The extraction recovery of the five analytes was 97.6—105.6% and the RSD values were < 2.0% The relative standard deviation values of intra- and interday precision for all analytes were < 1.71 and < 1.46%, respectively. As determined using the established and validated HPLC-PDA method described here, the amounts of the five marker compounds in M firmum were 0.02–2.54 mg/g.


2021 ◽  
Vol 19 (1) ◽  
pp. 205-213
Author(s):  
Hany W. Darwish ◽  
Abdulrahman A. Al Majed ◽  
Ibrahim A. Al-Suwaidan ◽  
Ibrahim A. Darwish ◽  
Ahmed H. Bakheit ◽  
...  

Abstract Five various chemometric methods were established for the simultaneous determination of azilsartan medoxomil (AZM) and chlorthalidone in the presence of azilsartan which is the core impurity of AZM. The full spectrum-based chemometric techniques, namely partial least squares (PLS), principal component regression, and artificial neural networks (ANN), were among the applied methods. Besides, the ANN and PLS were the other two methods that were extended by genetic algorithm procedure (GA-PLS and GA-ANN) as a wavelength selection procedure. The models were developed by applying a multilevel multifactor experimental design. The predictive power of the suggested models was evaluated through a validation set containing nine mixtures with different ratios of the three analytes. For the analysis of Edarbyclor® tablets, all the proposed procedures were applied and the best results were achieved in the case of ANN, GA-ANN, and GA-PLS methods. The findings of the three methods were revealed as the quantitative tool for the analysis of the three components without any intrusion from the co-formulated excipient and without prior separation procedures. Moreover, the GA impact on strengthening the predictive power of ANN- and PLS-based models was also highlighted.


2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Vaibhav S. Adhao ◽  
Suraj R. Chaudhari ◽  
Jaya P. Ambhore ◽  
Sunil Sangolkar ◽  
Raju R. Thenge ◽  
...  

Abstract Background Human immunodeficiency virus (HIV) causes severe life-threatening condition, i.e., AIDS. HIV destabilises an individual’s ability to prevent infection. Therefore, the combine medication lamivudine (LVD) and tenofovir disoproxil fumarate (TDF) are prescribed to suppress the amount of HIV infection in individual’s body; thus, the individual’s immune system could function properly. Consequently, the objective of present research work was to investigate robust and sensitive liquid chromatography avenue for simultaneous determination of lamivudine and tenofovir disoproxil fumarate in pure material and combined dosage form. Results The reversed-phase chromatographic separation has been performed through Hypersil BDS C18 column using solvent system composed of 10 mM potassium dihydrogen phosphate (pH 4.0): acetonitrile (60:40% v/v). The determination was executed at 30 oC at 1 mL/min rate for flow of solvent system through column. The eluents of column were monitored at 265 nm using Photodiode Array detector has revealed admirable retention times, i.e., 4.67 and 8.78 min for both drugs, respectively. The calibration curve demonstrated excellent linearity in the range of 10–50 μg/mL for lamivudine and tenofovir disoproxil fumarate with better determination coefficients was more than (r2 0.999). Conclusion The estimable method was effectively validated with respect to accuracy, precision, sensitive (limit of detection and limit of quantitation), robustness, ruggedness, and for selectivity and specificity. The value less than 2 for percentage relative standard deviation for accuracy, precision, robustness, and ruggedness satisfying the acceptance criteria as per procedure of International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use.


2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Shilan A. Omer ◽  
Nabil A. Fakhre

In this study, three simple and accurate spectrophotometric methods for simultaneous determination of pyriproxyfen and chlorothalonil residues in cucumbers and cabbages grown in experimental greenhouse were studied. The first method was based on the zero-crossing technique measurement for first and second derivative spectrophotometry. The second method was based on the first derivative of the ratio spectra. However, the third method was based on mean centering of ratio spectra. These procedures lack any previous separation steps. The calibration curves for three spectrophotometric methods are linear in the concentration range of 1–30 μg·mL−1 and 0.5–7 μg·mL−1 for pyriproxyfen and chlorothalonil successively. The recoveries ranged from 82.12–97.40% for pyriproxyfen and 81.51–97.04% for chlorothalonil with relative standard deviations less than 4.95% and 5.45% in all instances for pyriproxyfen and chlorothalonil, respectively. The results obtained from the proposed methods were compared statistically by using one-way ANOVA, and the results revealed there were no significant differences between ratio spectra and mean centering methods with the zero-crossing technique. The proposed methods are successfully applied for the simultaneous estimation of the residue of both pesticides in cucumber and cabbage samples.


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