scholarly journals Study on the Determination of Tauroursodeoxycholic Acid in Bear Bile Powder by HPLC-MS/MS

2021 ◽  
Vol 2 (2) ◽  
Author(s):  
Kaibin Huang ◽  
Wenbi Pan ◽  
Chuntian Yang ◽  
Yingying Ye ◽  
Xiaoce Lyu
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Ion Pairs ◽  
Negative Ion ◽  
Tauroursodeoxycholic Acid ◽  
Column Temperature ◽  
Bear Bile ◽  
Bear Bile Powder

Objective — To establish a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the rapid determination of tauroursodeoxycholic acid (TUDCA) in bear bile powder. Method — The chromatographic conditions were optimized. A Hypersil GOLD chromatographic column (Thermo Fisher, 100 mm×2.1 mm) was used with the mobile phase of methanol:water (0.1mmol/l ammonium acetate + 0.1% formic acid) = 75:25 for isocratic elution; the column temperature is 30.0℃; the flow rate is 0.2mL/min; the injection volume is 5uL; the negative ion scanning mode and the select reaction monitoring are used. Through the compound optimization function of the instrument, the two characteristic ion pairs of TUDCA are m/z: 498.5/124.0 and m/z: 498.5/79.8 (quantitative ion pair). Results — The detection limit of this method was 5ng/mL, and the linear range was 20~1000ng/mL (r=0.9993). The same sample was measured in parallel with the high performance liquid chromatography (HPLC/UV) method, and the analysis results were basically the same. Conclusion — Compared with HPLC/UV, HPLC-MS/MS is simple, more sensitive and accurate for the determination of TUDCA in bear bile powder. The method can be used in the quality assessment and process control of bear bile powder.

Comparison Study on the Contents of Eight Flavonoids in three Different Processed Products of Scutellariae Radix using Ultra-high Performance Liquid Chromatography Coupled With Triple-Quadrupole Mass Spectrometry

2020 ◽  
Vol 16 (6) ◽  
pp. 690-697
Author(s):  
Yuedong Yang ◽  
Hao Zhi ◽  
Baofei Yan ◽  
Yi Tian ◽  
Jianping Shen ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
High Performance ◽  
Triple Quadrupole ◽  
Column Temperature ◽  
Scutellariae Radix ◽  
Total Percentage

Background: The simultaneous determination of multiple components in a sample is an important factor in the quality control of traditional Chinese medicines and can give an indication of potential clinical applications. Introduction: A rapid and sensitive method has been introduced for the simultaneous quantitative analysis of eight bioactive flavonoid constituents from Scutellariae Radix using ultra-high performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry. Methods: The separation was performed on a Waters Acquity UPLC C18 column (2.1 mm×100 mm, 1.7 μm), under optimized mass spectrometry conditions, with a flow rate of 0.3 mL/min. The column temperature was maintained at 35°C and the injection volume was 3 μL. Results: The method showed a good linear relationship of each component; all R2 values were above 0.9990 in the experiment. The RSDs of the precision test, repeatability test, stability test and recovery test were all not more than 2.86 %. We found that the total percentage amounts of the eight flavonoids were 22.19%, 18.63% and 10.86% in Raw Scutellariae Radix (RSR), Wine Scutellaria Radix (WSR) and Scutellaria Radix Charcoal (SRC) respectively. Conclusion: The method was successfully applied to the simultaneous determination of the eight bioactive flavonoids of Raw Scutellariae Radix, Wine Scutellaria Radix and Scutellaria Radix Charcoal.

scholarly journals Simultaneous Determination of Nine Bioactive Constituents of Caulis Lonicerae Japonicae by High-Performance Liquid Chromatography Coupled with Mass Spectrometry

2008 ◽  
Vol 3 (5) ◽  
pp. 1934578X0800300 ◽  
Author(s):  
Hui-Jun Li ◽  
Zheng-Ming Qian ◽  
Ping Li ◽  
Mei-Ting Ren ◽  
Jun Chen ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
High Performance ◽  
Limit Of Detection ◽  
Quinic Acid ◽  
Column Temperature ◽  
Caffeoyl Quinic Acid

A new high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS) method has been developed for the simultaneous determination of nine major compounds, namely chlorogenic acid (1), caffeic acid (2), sweroside (3), loganin (4), secoxyloganin (5), 3,5-di- O-caffeoyl quinic acid (6), luteolin-7- O-glucoside (7), rutin (8) and 3,4-di- O-caffeoyl quinic acid (9), in Caulis Lonicerae Japonicae (CLJ), a commonly used traditional Chinese medicinal herb. The separation was achieved on a C-18 column (250 × 4.6 mm, 5.0 μm) with a column temperature of 30°C and a flow-rate of 0.8 mL/min. The mobile phase was composed of (A) aqueous formic acid (0.1%, v/v) and (B) methanol, using a gradient elution of 30% B for 0-13 min, 30–40% B for 13–17 min, and 40–49% B for 17–30 min. The limit of detection ( S/ N = 3) ranged from 0.8 to 5.1 ng/mL and the limit of quantification ( S/ N = 10) varied from 3.4 to 16.9 ng/mL. All calibration curves showed good linear regression ( r2 > 0.9976) within the test ranges. The intra- and inter-day precisions, as determined from sample solutions, were below 2.2 and 4.3%, respectively. The recoveries for nine compounds were within 91.3 and 104.2%. This proposed method has been successfully applied to evaluation of commercial samples of CLJ from different markets in China, which provides a new basis of assessment of the quality of the herbal drug.

scholarly journals Determination of Benzalkonium Chloride in Nasal Drops by High-Performance Liquid Chromatography

2012 ◽  
Vol 9 (3) ◽  
pp. 1599-1604 ◽  
Author(s):  
Danijela A. Kostić ◽  
Snezana S. Mitić ◽  
Danijela Č. Nasković ◽  
Aleksandra R. Zarubica ◽  
Milan N. Mitic
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Benzalkonium Chloride ◽  
High Performance ◽  
Reversed Phase ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Acceptance Range

A high-performance liquid chromatography (HPLC) system was used in the reversed phase mode for the determination of benzalkonium chloride (BKC) in nosal drops. A Chromolit RP-18e, 100 x 4.6, (UM6077/035) column was used at 40 °C. The mobile phase, optimized through an experimental design, was a 70:30 (v/v) mixture of 0.057M Na-heksansulphonate potassium, dihydrogen orthophosphate buffer (pH 2.9) and acetonitrile, pumped at a flow rate of 1.75 mL/min at maintaining column temperature at 40 °C. Maximum UV detection was achieved at 215 nm. The method was validated in terms of selectivity, linearity, repeatability, precision and accuracy. The method was successfully applied for the determination of BKC in a pharmaceutical formulation of nasal drop solution without any interference from common excipients and drug substance. All the validation parameters were within the acceptance range, concordant to ICH guidelines.

scholarly journals Determination of Ketotifen Fumarate in Syrup Dosage Form by High Performance Liquid Chromatography

2020 ◽  
pp. 63-72
Author(s):  
Mohammed Ali Salih ◽  
Dlivan Fattah Aziz ◽  
Salar Ibrahim Ali
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Column Temperature ◽  
Ketotifen Fumarate ◽  
Suggested Technique ◽  
Elution Method

The goal of the current study was to establish and authenticate an isocratic reverse-stage High-Performance Liquid Chromatography (HPLC) method for quantifying ketotifen fumarate (KF) in pharmaceutical liquid dosage compositions. Easy, quick, accurate, exact, and accurate reverse-stage high-performance liquid chromatography was advanced for the simultaneous assessment of ketotifen fumarate in the liquid syrup dosage type. The HPLC system using isocratic elution method with reverse-phase Inertsil ODS-(250 mm × 4.6 mm, 3 μm) column was detected by ultraviolet absorbance at 297 nm with no interference from widely using excipients, the mobile phase (A) is a mixture of triethylamine and water (175 μl in 500 ml of water), and the mobile phase (B) is a mixture of triethylamine and methanol (175 μl in 500 ml of methanol) at a flow rate of 1.5 mL/min (mobile phase A 40 %:mobile phase B 60%) at column temperature using 40 ° C, the retention time for ketotifen fumarate was 6.4±0.5 min. The concentration curves were linear in the range of 10.0 to 35.0 μg / ml (R2 = 0.9999). The developed method was tested for the specificity, precision, linearity, precision, reliability, robustness, and consistency of the solution. The regeneration of ketotifen fumarate in formulations was found to be 99.75 %, 99.91 %, and 100.05 % respectively. The percent RSD for percent recovery was found to be 0.21 and 0.17 and 0.10 for ketotifen fumarate. In the conclusion, the suggested technique was successfully used for the quantitative determination of ketotifen fumarate in formulations.

scholarly journals Simultaneous Determination Of Six Parabens In Cosmetics By A New High Performance Liquid Chromatography Method With Fluorescence Detection

2020 ◽  
Vol 15 (1) ◽  
pp. 27-32
Author(s):  
Pelin Kцseoğlu Yılmaz ◽  
Mehmet Akif Tokat
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Fluorescence Detection ◽  
High Performance ◽  
Water Mixture ◽  
Chromatography Method ◽  
Column Temperature ◽  
Liquid Chromatography Method

In this study, a new high performance liquid chromatography method with fluorescence detection was developed and validated for the simultaneous determination of methyl paraben, ethyl paraben, propyl paraben, isopropyl paraben, butyl paraben and benzyl paraben in cosmetics. Separations were achieved using a C18 guard column (2.1 Ч 10 mm, 3 µm) and a C18 analytical column (2.1 Ч 150 mm, 3 µm). Isocratic elution was applied with a mobile phase consisting of 45 % aqueous o-phosphoric acid solution (0.08 %) and 55 % methanol/water mixture (90 : 10 v/v). The excitation and the emission wavelengths were 254 and 310 nm, respectively. Column temperature was fixed at 40 єC. The linear range was 0.50-10.00 μg/mL for all of the parabens. Limits of detection and quantification were in the range of 0.29-0.32 μg/mL and 0.88-0.97 μg/ mL, respectively. Precision and accuracy values were calculated by analysis results of standard solutions at 0.50, 2.50 and 10.00 μg/mL. The developed and validated method was applied for simultaneous quantitative determination of six paraben species in cosmetic tonic and micellar water samples successfully.

scholarly journals Chromatographic Method for Determination of the Amino Acid Content in Dioscorea bulbifera L. Tubers by RP-HPLC

2019 ◽  
Vol 25 (1) ◽  
pp. 65-69 ◽  
Author(s):  
Musadiq Hussain Bhat ◽  
Mufida Fayaz ◽  
Amit Kumar ◽  
Alamgir Ahmad Dar ◽  
Ashok Kumar Jain
Keyword(s):  
Amino Acids ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Amino Acid ◽  
Acid Content ◽  
High Performance ◽  
Amino Acid Content ◽  
Column Temperature ◽  
Dioscorea Bulbifera

Background: The present study was carried out for determination of amino acid content in tubers of Dioscorea bulbifera using reverse-phase high-performance liquid chromatography. Methods: The method involved the vapor phase hydrolysis of the sample, automated derivatisation of the amino acids with the aid of AccQ-Fluor reagent kit, separated on a high performance liquid chromatography equipped with photo diode array (HPLC-PDA) at 254 nm having column temperature of 37 ºC. Results: The proportional molar concentration for each amino acid was calculated based on the concentration of standard amino acids and expressed as μg amino acid/mg sample. Methionine, aspartic acid and leucine were major components while as tyrosine was found minor from the plant on dry weight basis. Conclusion: The method is reliable, simple and economical for determining the amino acid content of Dioscorea bulbifera tubers.

Chiral Resolution and Content Determination of Ketorolac Tromethamine Using High-performance Liquid Chromatography

2020 ◽  
Vol 17 ◽  
Author(s):  
Lei Zheng ◽  
Jing Yang ◽  
Yu-yao Guan ◽  
Lei Zhang ◽  
Chao Song ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Hplc Method ◽  
Chiral Resolution ◽  
Ketorolac Tromethamine ◽  
Column Temperature ◽  
Relative Standard ◽  
Determination Methods

Background:: Establishing R, S-enantiomer (S-KT and R-KT) chiral resolution and determination methods for KT are of great significance. Objective:: This study aimed to establish a high-performance liquid chromatography (HPLC) method for the resolution and determination of ketorolac tromethamine (KT) enantiomers. Methods:: A CHIRALPAK AGP column (0.4  10 cm, 5 μm) was used with 10 mmol/L ammonium acetate (pH 5.5) and isopropanol (97:3) as the mobile phase. The detection wavelength was 324 nm, the flow rate was 1.0 mL/min, the column temperature was 25°C, and the injection volume was 5 μL. Results:: The resolution between S-KT and R-KT was 2.8. S-KT and R-KT demonstrated a good linear relationship in the range of 3-60 μg/mL (r > 0.999). The average recoveries of S-KT and R-KT were 99.2% and 99.8%, with relative standard deviations of 2.0% and 2.4%, respectively. Conclusion:: The established method can be used for the resolution and determination of S-KT and R-KT.

scholarly journals RP-LC and TLC Densitometric Determination of Paracetamol and Pamabrom in Presence of Hazardous Impurity of Paracetamol and Application to Pharmaceuticals

2013 ◽  
Vol 8 ◽  
pp. ACI.S12349 ◽  
Author(s):  
Ola Mohamed El-Houssini
Keyword(s):  
High Performance Liquid Chromatography ◽  
Acetic Acid ◽  
Liquid Chromatography ◽  
Thin Layer ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Column Temperature ◽  
Layer Chromatography

Two simple, accurate and reproducible methods were developed and validated for the simultaneous determination of paracetamol (PARA) and pamabrom (PAMB) in pure form and in tablets. The first method was based on reserved-phase high-performance liquid chromatography, on a Thermo Hypersil ODS column using methanol:0.01 M sodium hexane sulfonate:formic acid (67.5:212.5:1 v/v/v) as the mobile phase. The flow rate was 2 mL/min and the column temperature was adjusted to 35 °C. Quantification was achieved with UV detection at 277 nm over concentration range of 100-600 and 4-24 μg/mL, with mean percentage recoveries were found to be 99.90 ± 0.586 and 99.26 ± 0.901 for PARA and PAMB, respectively. The second method was based on thin-layer chromatography separation of PARA and PAMB followed by densitometric measurement of the spots at 254 nm and 277 nm for PARA and PAMB respectively. Separation was carried out on aluminum sheet of silica gel 60F254 using dichloromethane:methanol:glacial acetic acid (7.5:1:0.5 v/v/v) as the mobile phase over concentration range of 1-10 and 0.32-3.20 μg per spot, with mean percentage recovery of 100.52 ± 1.332 and 99.71 ± 1.478 for PARA and PAMB, respectively. The methods retained their accuracy in presence of up to 50% of P-aminophenol and could be successfully applied in tablets.

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