scholarly journals Analysis of Non-Ionic Surfactant Triton X-100 Using Hydrophilic Interaction Liquid Chromatography and Mass Spectrometry

Molecules ◽  
2019 ◽  
Vol 24 (7) ◽  
pp. 1223 ◽  
Author(s):  
Evelin Farsang ◽  
Violetta Gaál ◽  
Ottó Horváth ◽  
Erzsébet Bárdos ◽  
Krisztián Horváth
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Performance ◽  
Gradient Elution ◽  
Water Soluble ◽  
Ionic Surfactant ◽  
Hydrophilic Interaction ◽  
Retention Model ◽  
Mass Unit ◽  
Triton X

It is well known that surfactants increase the solubility of hydrophobic organic compounds and cause adverse environmental effects. The removal of these compounds from the contaminated soil or ground-water is particularly difficult due to their water soluble feature. In this work, an ultra-high performance hydrophilic interaction liquid chromatographic method was developed for the separation of oligomers of Triton X-100 octylphenol-polyethoxylate non-ionic surfactant. Liquid chromatography-mass spectrometry (LC-MS) was used to identify the Triton X-100 compounds. There was a 44 mass unit difference between two adjacent peaks that is the molar mass of one ethylene oxide group (–CH 2 CH 2 O–). A quadratic retention model was applied for the estimation of retention of the examined non-ionic surfactant and the optimization of gradient elution conditions. The optimized method was suitable for the baseline separation of 28 Triton X-100 oligomers in five minutes.

scholarly journals Determination of Antiviral Drugs and Their Metabolites Using Micro-Solid Phase Extraction and UHPLC-MS/MS in Reversed-Phase and Hydrophilic Interaction Chromatography Modes

Molecules ◽  
2021 ◽  
Vol 26 (8) ◽  
pp. 2123
Author(s):  
Luboš Fical ◽  
Maria Khalikova ◽  
Hana Kočová Vlčková ◽  
Ivona Lhotská ◽  
Zuzana Hadysová ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Tandem Mass ◽  
Phase Extraction ◽  
Hydrophilic Interaction

Two new ultra-high performance liquid chromatography (UHPLC) methods for analyzing 21 selected antivirals and their metabolites were optimized, including sample preparation step, LC separation conditions, and tandem mass spectrometry detection. Micro-solid phase extraction in pipette tips was used to extract antivirals from the biological material of Hanks balanced salt medium of pH 7.4 and 6.5. These media were used in experiments to evaluate the membrane transport of antiviral drugs. Challenging diversity of physicochemical properties was overcome using combined sorbent composed of C18 and ion exchange moiety, which finally allowed to cover the whole range of tested antivirals. For separation, reversed-phase (RP) chromatography and hydrophilic interaction liquid chromatography (HILIC), were optimized using extensive screening of stationary and mobile phase combinations. Optimized RP-UHPLC separation was carried out using BEH Shield RP18 stationary phase and gradient elution with 25 mmol/L formic acid in acetonitrile and in water. HILIC separation was accomplished with a Cortecs HILIC column and gradient elution with 25 mmol/L ammonium formate pH 3 and acetonitrile. Tandem mass spectrometry (MS/MS) conditions were optimized in both chromatographic modes, but obtained results revealed only a little difference in parameters of capillary voltage and cone voltage. While RP-UHPLC-MS/MS exhibited superior separation selectivity, HILIC-UHPLC-MS/MS has shown substantially higher sensitivity of two orders of magnitude for many compounds. Method validation results indicated that HILIC mode was more suitable for multianalyte methods. Despite better separation selectivity achieved in RP-UHPLC-MS/MS, the matrix effects were noticed while using both chromatographic modes leading to signal enhancement in RP and signal suppression in HILIC.

scholarly journals Chemical Profiles and Simultaneous Quantification of Aurantii fructus by Use of HPLC-Q-TOF-MS Combined with GC-MS and HPLC Methods

Molecules ◽  
2018 ◽  
Vol 23 (9) ◽  
pp. 2189 ◽  
Author(s):  
Yingjie He ◽  
Zongkai Li ◽  
Wei Wang ◽  
Suren Sooranna ◽  
Yiting Shi ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Quality Control ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Gradient Elution ◽  
Chemical Components ◽  
Bioactive Substances ◽  
Flight Mass Spectrometry ◽  
Tof Ms

Aurantii fructus (AF) is a traditional Chinese medicine that has been used to improve gastrointestinal motility disorders for over a thousand years, but there is no exhaustive identification of the basic chemical components and comprehensive quality control of this herb. In this study, high-performance liquid chromatography coupled with quadrupole time of flight mass spectrometry (HPLC-Q-TOF-MS) and gas chromatography coupled mass spectrometry (GC-MS) were employed to identify the basic chemical compounds, and high-performance liquid chromatography (HPLC) was developed to determine the major biochemical markers from AF extract. There were 104 compounds belonging to eight structure types, including 13 amino acids or peptides, seven alkaloids, 18 flavanones, 14 flavones, 15 polymethoxyflavonoids, six triterpenoids, nine coumarins, and 18 volatile oils, as well as four other compounds that were systematically identified as the basic components from AF, and among them, 41 compounds were reported for the first time. Twelve bioactive ingredients were chosen as the benchmark markers to evaluate the quality of AF. The analysis was completed with a gradient elution at a flow rate of 0.7 mL/min within 55 min. This efficient method was validated showing good linearity, precision, stability, repeatability and recovery. Furthermore, the method was successfully applied to the simultaneous determination of 12 chemical markers in different samples of AF. This study could be applied to the identification of multiple bioactive substances and improve the quality control of AF.

EVIDENCE FOR BIIIARY EXCRETION OF PHENPROCOUMON AND ITS METABOLITES IN HUMANS; IDENTIFICATION BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY AND GAS CHROMATOGRAPHY-MASS SPECTROMETRY

1987 ◽  
Author(s):  
J X de Vries ◽  
R Raedsch ◽  
A Stiehl ◽  
U Voelker ◽  
I Walter-Sack ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Gradient ◽  
Chromatography Mass Spectrometry

Recently it has been shown that in man the oral couma-rin anticoagulant phenprocoumon is eliminated up to 60-70 % in urine and 30-40 % in faeces; in urine phenprocoumon (PH) and its metabolites 7-hydroxy-(7-OH),6-hydroxy-(6-OH) and 4'-hydroxy-(4'-OH) phenprocoumon are present mainly as conjugates. No data so far were available on the biliary excretion of these compounds.We examined bile obtained from four in-patients during PH treatment; bile samples were aspirated in the duodenum at the papilla during routine diagnostic endoscopy and immediately deep frozen before analysis. Samples were extracted both untreated as well as after hydrolysis with 6-glucuronidase/aryl sulfatase and separated by reversed phase gradient elution high performance liquid chromatography (HPLC) with fluorescence detection; for confirmation, the same extracts were methylated and analysed by gas chromatography-mass spectrometry (CG-MS) (J.X.de Vries et al J Chromatogr., 338 (1985) 325). PH, 7-OH, 6-OH and 4'-OH were identified by comparison with synthetic authentic samples'''''''

scholarly journals Levoglucosan concentrations in ice-core samples from the Tibetan Plateau determined by reverse-phase high-performance liquid chromatography–mass spectrometry

2013 ◽  
Vol 59 (216) ◽  
pp. 599-612 ◽  
Author(s):  
Ping Yao ◽  
Valérie F. Schwab ◽  
Vanessa-Nina Roth ◽  
Baiqing Xu ◽  
Tandong Yao ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Tibetan Plateau ◽  
Biomass Burning ◽  
High Performance ◽  
Ice Core ◽  
Water Soluble ◽  
The Tibetan Plateau ◽  
Core Samples

AbstractLevoglucosan is a unique marker for biomass burning that can be transported in the atmosphere and preserved in archives such as ice cores. A new method to determine the concentrations of levoglucosan in Tibetan ice-core samples using high-performance liquid chromatography with electrospray ionization mass spectrometry (HPLC-ESI/MS) was developed. Levoglucosan was separated from coeluting water-soluble organic compounds using a C18 column with a gradient program from 50% to 90% methanol in ultrapure water. An external standard calibration curve (R2 = 0.9958) was established by plotting the ion m/z 163 [M+H]+ peak area versus the amount of analyte. The repeatability ranges between 11% and 2% at a concentration around 10 and 150 ng mL−1. The limit of detection was 10 ng mL−1 and the limit of quantification was 40 ng mL−1. Levoglucosan concentrations ranged from 10 to 718 ng mL−1 in the Muztagh Ata ice core and from 10 to 93 ng mL−1 in the Tanggula ice core. These concentrations, up to 1000 times higher than those measured in samples from Antarctic and Greenland, showed the higher vulnerability of the Tibetan Plateau glaciers to biomass burning events.

scholarly journals Method Development and Validation for Quantification of Potential Genotoxic Impurity, PyCl in Lansoprazole Hydrochloride using Liquid Chromatography Combined with Mass Spectrometry

2021 ◽  
Vol 33 (5) ◽  
pp. 1165-1168
Author(s):  
C. Purushotham Reddy ◽  
G. Venkateswara Rao ◽  
K. Ramakrishna ◽  
K.M.V. Narayana Rao
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Solution Stability ◽  
Selective Ion Monitoring ◽  
Acquity Uplc

A sensitive and robust high performance liquid chromatography combined with tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of potential genotoxic impurity (PGI), 2-(chloromethyl)-3-methyl-4-(2,2,2-trifluoroethoxy)-pyridine hydrochloride (PyCl) in lansoprazole as per ICH Q2 guideline. In this method, PyCl and lansoprazole were well-separated from each other on Acquity UPLC BEH-C18 column (50 × 4.6 mm × 1.7 μ) in a gradient elution mode with the mobile phase consisting of 0.1% formic acid in water (mobile phase-A) and acetonitrile (mobile phase-B) at a flow rate of 0.4 mL/min. For the quantitation of Py-Cl, selective ion monitoring (SIM) mode was used with m/z 240 ion in LC-MS method. The validated method was found to be precise, accurate and linear from the range of LOQ level to 150% with respect to sample concentration and the correlation co-efficient was found to be 0.998. Limit of detection (LOD) and limit of quantifications (LOQ) were found to be 0.000012 and 0.000004 mg/mL, respectively. The validated method was found to be sensitive and the recoveries were found to be well within the range from 83.4% to 95.9% for Py-Cl. Further, the solution stability was also established as the same were found to be stable upto 24 h.

scholarly journals An Analytical Method to Screen for Six Thyreostatic Drug Residues in the Thyroid Gland andMuscle Tissues of Food Producing Animals by Liquid Chromatography with Ultraviolet Absorption Detection and Liquid Chromatography/Mass Spectrometry

2006 ◽  
Vol 89 (2) ◽  
pp. 567-575 ◽  
Author(s):  
Philip E Asea ◽  
James D MacNeil ◽  
Joe O Boison
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Performance ◽  
Solid Phase ◽  
Thyroid Tissue ◽  
Internal Standard ◽  
Gradient Elution ◽  
Internal Standards ◽  
Tissue Samples ◽  
Muscle Tissues

Abstract A method was developed and validated to screen for residues of the thyreostatic drugs, tapazole (TAP), mercaptobenzimidazole (MBI), thiouracil (TU), methylthiouracil (MTU), propylthiouracil (PrTU), and phenylthiouracil (PhTU) in bovine, equine, ovine, and porcine thyroid and muscle tissues at concentrations 5 ng/g using 2-methoxy-mercaptobenzimidazole (MeMBI) and dimethylthiouracil (DMTU) as internal standards. In this method, the drugs were solvent extracted from thyroid and muscle tissue and cleaned up on an amino-propyl solid-phase extraction (SPE) cartridge. The unretained fraction containing TAP and MBI and the internal standard, MeMBI, was collected as Fraction 1. The retained fraction containing TU, MTU, PrTU, PhTU, and the internal standard, DMTU, was eluted with 3 acetic acidisopropanol as Fraction 2. Fraction 1 was further cleaned up on an alumina B SPE cartridge and analyzed by gradient elution on a C18 high-performance liquid chromatography (HPLC) column with ultraviolet detection at wavelengths of 255 and 300 nm. Fraction 2 was taken to dryness, derivatized with 4-chloro-7-nitrobenzo-2-furazan at pH 8, and analyzed by gradient elution on a C18 LC column with mass spectrometry (MS) detection. Any presumptive positive test results were submitted for further analysis by LC/MS/MS. The validated method was applied to the analysis of over 300 thyroid tissue samples.

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