A Powerful HPLC-ELSD Method for Simultaneous Determination of Fecal Bile Acids in T2DM Rats Interfered by Sanhuang Xiexin Tang

2021 ◽  
Author(s):  
Mengjun Chen ◽  
Chen Liu ◽  
Yumeng Shen ◽  
Junfeng Zou ◽  
Zhimiao Zhang ◽  
...  
Keyword(s):  
Bile Acids ◽  
Simultaneous Determination ◽  
High Performance ◽  
Farnesoid X Receptor ◽  
Glycolipid Metabolism ◽  
Fecal Bile Acids ◽  
Mobile Phases ◽  
Evaporative Light Scattering ◽  
Relative Standard

Abstract Bile acids (BAs) as important endogenous ligands can activate farnesoid X receptor (FXR) and G-protein-coupled bile acid receptor 1 (GPBAR1, also known as TGR5) signaling to regulate glycolipid metabolism. In this study, a simple, reliable and sensitive analysis method for simultaneous determination of four BAs from rat feces based on high-performance liquid chromatography with evaporative light scattering detector (HPLC-ELSD) was developed. Chromatographic analysis was performed with the mobile phases of acetonitrile and 0.2% formic acid. All the standard curves exhibited good linearity (R2 ≥ 0.99). The relative standard deviations of precision, stability and repeatability varied from 1.27 to 3.96%, 2.20 to 3.89% and 3.00 to 4.31%, respectively. The validated method was successfully applied to investigate the variation of four BAs in feces from T2DM rats after oral administration of Sanhuang Xiexin Tang (SXT). Data showed that SXT could remarkably increase the contents of conjunct BAs and decrease the contents of free BAs, which might contribute to ameliorate the symptoms of T2DM rats.

Simultaneous Determination of Eight New Generation Amide Insecticide Residues in Complex Matrix Agri-food by Multi-walled Carbon Nanotube Cleanup and UPLC-MS/MS

2021 ◽  
Author(s):  
Tao Lin ◽  
Xinglian Chen ◽  
Li Wang ◽  
Haixian Fang ◽  
Maoxuan Li ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Simultaneous Determination ◽  
High Performance ◽  
Rapid Determination ◽  
Complex Matrix ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
The Matrix ◽  
Multi Walled Carbon Nanotubes

Abstract The simultaneous determination method of 8 amide pesticides by multi-walled carbon nanotubes (MWCNs) cleanup, combined with QuEChERS method and ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry has been developed and successfully applied in complex matrix such as green onions, celery, leeks, citrus, lychees, avocado. The matric effect of MWCNs is optimized and compared with QuEChERS materials. The results show that MWCNs can effectively reduce the matrix effect in sample extraction. The mass spectrometry is optimized, through their chemical structure skeletons, the ESI+ and ESI- mode are simultaneously scanned in the method. The coefficient (r) is greater than 0.9990, the limit of quantification ranges from 0.03 to 0.80 μg/kg, the recovery rate ranges from 71.2% to 120%, and the relative standard deviation (RSD) ranges from 3.8% to 9.4%. The method is fast, simple, sensitive, and has good purification effect. It is suitable for the rapid determination of amide pesticides in complex matrix agri-food.

scholarly journals Development and Validation of a Reversed-Phase High-Performance Liquid Chromatographic Method for the Simultaneous Determination of Amiloride Hydrochloride, Atenolol, Hydrochlorothiazide, and Chlorthalidone in Their Combined Mixtures

2009 ◽  
Vol 92 (2) ◽  
pp. 404-409 ◽  
Author(s):  
Abdalla A Elshanawane ◽  
Samia M Mostafa ◽  
Mohamed S Elgawish
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Chromatographic Method ◽  
High Performance Liquid Chromatographic ◽  
Ternary Mixtures ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic ◽  
Amiloride Hydrochloride

Abstract A high-performance liquid chromatographic method was developed for the simultaneous determination of 2 ternary mixtures containing amiloride hydrochloride, atenolol, hydrochlorothiazide, and chlorthalidone used in hypertension therapy. The use of cyanopropyl column results in satisfactory separation of both mixtures. The mobile phase consisted of 10 mM KH2PO4 buffer (pH 4.5) and methanol in a ratio of (75 25 v/v), at a flow rate of 1 mL/min. UV detector was operated at 275 nm. Calibration graphs were linear in the concentration ranges of 210, 20200, 10100, and 550 g/mL for amiloride hydrochloride, atenolol, hydrochlorothiazide, and chlorthalidone, respectively. Intraday and interday precision values (relative standard deviation) were <1.13 for mixture I (amiloride hydrochloride, atenolol, chlorthalidone), and <0.93 for mixture II (amiloride hydrochloride, atenolol, hydrochlorothiazide). The method was successfully applied for the determination of the 2 combinations in laboratory-prepared mixtures and commercial pharmaceutical formulation with high accuracy and precision. Statistical comparison of the results with those of the published methods showed excellent agreement and indicates no significant difference between them.

scholarly journals Development and Validation of a HPLC–PDA Method for the Simultaneous Determination of Berberine, Palmatine, Geniposide, and Paeoniflorin in Haedoksamul-tang

2020 ◽  
Vol 10 (16) ◽  
pp. 5482
Author(s):  
Beom-Geun Jo ◽  
Kyung-Hwa Kang ◽  
Min Hye Yang
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Array Detector ◽  
Column Temperature ◽  
Gardenia Jasminoides ◽  
Photodiode Array Detector ◽  
Relative Standard ◽  
Marker Compounds ◽  
Development And Validation

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.

Simultaneous Determination of Phenolic Acids, Anthraquinones, and Flavonoids in the Aerial Part and the Fruit of Xanthium Sibiricum by LC- ESI- QTRAP-MS/MS

2019 ◽  
Vol 15 (5) ◽  
pp. 542-553
Author(s):  
Hui Zhao ◽  
Hao Cai ◽  
Juan-Xiu Liu ◽  
Sheng-Nan Wang ◽  
Xun-Hong Liu ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Phenolic Acids ◽  
High Performance ◽  
Aerial Part ◽  
Multiple Reaction Monitoring ◽  
Principal Component ◽  
Negative Ion ◽  
Xanthium Sibiricum ◽  
Relative Standard

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.

A Rapid and Sensitive HPLC-FLD Method for the Determination of Retinol and Vitamin E Isomers in Human Serum

2019 ◽  
Vol 15 (7) ◽  
pp. 745-752
Author(s):  
Yi Yang ◽  
Dan Lu ◽  
Danni Yang ◽  
Shuo Yin ◽  
Jing Zhang ◽  
...  
Keyword(s):  
Vitamin E ◽  
Human Serum ◽  
Simultaneous Determination ◽  
Fluorescence Detection ◽  
High Performance ◽  
Correlation Coefficients ◽  
Serum Samples ◽  
Rapid Separation ◽  
Relative Standard

Background: Retinol and vitamin E are fat-soluble vitamins crucial for human health, yet their isomers’ distributions in the human body are still known roughly. In order to figure out the physical condition and evaluate the nutritional status of an individual, it is imperative to analyze retinol and VE isomers in human serum. Objective: This work aims to establish a rapid and simple high-performance liquid chromatography with fluorescence detection for simultaneous determination of retinol and vitamin E isomers in human serum. Methods: Separation was accomplished on a common C18 column thermostated at 25 oC, using a simple isocratic elution program of methanol/acetonitrile (85:15, v/v) at a flow rate of 1.0 mL/min. Fluorescence detection was operated using excitation/emission wavelengths of 329 nm/472 nm for retinol and 294 nm/338 nm for VE isomers, respectively. Results: Rapid separation was achieved within 13 min. Linear ranges of the method were 0.020-50.0 µg/mL, with correlation coefficients greater than 0.999. Detection limits and the quantification limits were 0.001-0.004 µg/mL and 0.003- 0.013 µg/mL, respectively. Mean recoveries were 84.1%- 98.2%, with intra-day and inter-day relative standard deviations less than 12.3% and 13.6%, respectively. This method has been applied to the simultaneous determination of retinol and 8 VE isomers in human serum samples with satisfactory results. Conclusion: A rapid, simple and robust method was developed for routine analysis of retinol and eight vitamin E isomers in human serum, providing a useful tool for clinical diagnosis and nutritional evaluation.

scholarly journals Simple and rapid liquid chromatography method for simultaneous determination of isoniazid and pyrazinamide in plasma

2012 ◽  
Vol 9 (1) ◽  
pp. 13-18 ◽  
Author(s):  
AK Kumar Hemanth ◽  
V Sudha ◽  
G Ramachandran
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Small Sample Size ◽  
Accurate Method ◽  
Reversed Phase ◽  
Small Sample ◽  
Pharmacokinetic Studies ◽  
Chromatography Method ◽  
Relative Standard

Introduction: Treatment of tuberculosis (TB) requires a combination of drugs. Isoniazid (INH) and pyrazinamide (PZA) are key components of the fi rst-line regimen used in the treatment of TB and monitoring these drug levels in plasma would help in better patient care. The objective of the study is to develop and validate a simple and rapid high performance liquid chromatographic method for simultaneous determination of INH and PZA in human plasma. Methodology: The method involved deproteinisation of plasma with para hydroxy benzaldehyde and trifl uoroacetic acid and analysis using a reversed-phase C8 column and UV detection at 267nm. The fl ow rate was set at 1.5 ml/min at ambient temperature. The accuracy, linearity, precision, specifi city, stability and recovery of the method were evaluated. The method was applied to estimate plasma INH and PZA collected from six children with TB. Results: Well resolved peaks of PZA and INH at retention times of 3.2 and 6.1 minutes respectively were obtained. The assay was linear from 0.25 - 10.0 ìg/ml for INH and 1.25 – 50.0 ìg/ml for PZA. The within-day and between-day relative standard deviation for standards were below 10%. The average recoveries of INH and PZA from plasma were 104 and 102% respectively. Conclusions: A rapid and accurate method for simultaneous determination of INH and PZA in plasma was validated. The assay spans the concentration range of clinical interest. The easy sample preparation and small sample size makes this assay highly suitable for pharmacokinetic studies of INH and PZA in TB patients. SAARC Journal of Tuberculosis, Lung Diseases & HIV/AIDS 2012; IX (1) 13-18 DOI: http://dx.doi.org/10.3126/saarctb.v9i1.6960

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