scholarly journals Ion-pairing chromatography and amine derivatization provide complementary approaches for the targeted UPLC-MS analysis of the polar metabolome

2021 ◽  
Author(s):  
Virag Sagi-Kiss ◽  
Yufeng Li ◽  
Matthew Carey ◽  
Sarah Grover ◽  
Karsten Siems ◽  
...  
Keyword(s):  
Ion Pairing ◽  
Reversed Phase ◽  
Triple Quadrupole Mass Spectrometer ◽  
Targeted Analysis ◽  
Coefficients Of Variation ◽  
Polar Metabolites ◽  
Phenol Compound ◽  
Phase Liquid ◽  
Combination Of Methods ◽  
Analytical Approaches

Liquid chromatography coupled to mass spectrometry is a key metabolomics technology. Reversed-phase liquid chromatog-raphy (RPLC) is very widely used as a separation step, possessing excellent characteristics with respect to reproducibility and reliability, but typically has poor retention of highly polar metabolites. Here, we evaluated the combination of two alter-native methods for improving retention of polar metabolites based on 6-aminoquinoloyl-N-hydroxysuccinidimyl carbamate derivatization for amine groups, and ion-pairing chromatography (IPC) using tributylamine as an ion-pairing agent to retain acids. We compared both of these methods to RPLC and also to each other, for targeted analysis using a triple-quadrupole mass spectrometer, applied to a library of ca. 500 polar metabolites. IPC and derivatization were complementary in terms of their coverage: combined, they improved the proportion of metabolites with good retention to 91%, compared to just 39% for RPLC alone. We detected 132 metabolites for real biological samples (liver extracts) with good reproducibility (based on coefficients of variation in pooled biological quality control samples). Finally, we tested the combination of methods with real-world samples by analyzing a set of liver extracts from aged male and female mice that had been treated with the poly-phenol compound ampelopsin. Furthermore, we also compared the results of these LC-MS methods to 1H NMR spectrosco-py as an orthogonal method (also termed statistical heterospectroscopy (SHY)), and found a strong correlation between the results of these different analytical approaches. By these means, not only were a number of significantly changed metabolites detected, but also it could be shown that there was a clear interaction between ampelopsin treatment and sex, in that the di-rection of metabolite change was opposite for males and females.

Targeted analysis of phenolic compounds by LC-MS v1

2021 ◽  
Author(s):  
Bashar Amer ◽  
Ramu Kakumanu ◽  
yangtian not provided ◽  
Aymerick Eudes ◽  
Edward EK Baidoo
Keyword(s):  
Phenolic Compounds ◽  
Plant Biomass ◽  
Reversed Phase ◽  
Industrial Applications ◽  
Liquid Chromatography Mass Spectrometry ◽  
Reversed Phase Liquid Chromatography ◽  
Sample Matrix ◽  
Targeted Analysis ◽  
Challenges And Opportunities ◽  
Phase Liquid

Cell-wall-bound (CWB) aromatics such as ferulate and p-coumarate play important physiological roles in plant development and response to stresses. Their presence also poses some challenges and opportunities during processing of plant biomass in various agro-industrial applications. To this end, we have developed a robust high-throughput reversed-phase liquid chromatography mass spectrometry method for quantifying CWB phenolic compounds. The method showed excellent linearity (R2 = ≥0.999) and intraday retention time repeatability (≤ 0.31 %RSD) for ferulate and p-coumarate. The limits of detection and quantitation for these analytes were ≤ 39 nM and 130 nM, respectively. Furthermore, there was very little effect of the CWB sample matrix on the retention times of the analytes and analyte percent recoveries from the CWB sample matrix was ≥83.91%.

Determination of nifedipine in serum or plasma by reversed-phase liquid chromatography.

1983 ◽  
Vol 29 (7) ◽  
pp. 1344-1348 ◽  
Author(s):  
P R Bach
Keyword(s):  
Liquid Chromatography ◽  
Reversed Phase ◽  
Extraction Column ◽  
Phase Extraction ◽  
Reversed Phase Liquid Chromatography ◽  
Ultraviolet Absorbance ◽  
Standard Curve ◽  
Coefficients Of Variation ◽  
Phase Liquid

Abstract Therapeutic concentrations of nifedipine in serum or plasma were measured by reversed-phase liquid chromatography, with detection by ultraviolet absorbance at 235 nm. In the procedure a disposable reversed-phase extraction column is used. A 1-mL sample is required. The method is sensitive to 3 micrograms of nifedipine per liter and the standard curve is linear to at least 400 micrograms/L. Coefficients of variation at 100 micrograms/L were 2.2% within-run, 2.8% between-run. The method has been used to determine nifedipine in patients involved in a test of its efficacy in treating muscular dystrophy.

Elimination of caffeine interference in HPLC determination of urinary nicotine and cotinine.

1989 ◽  
Vol 35 (7) ◽  
pp. 1456-1459 ◽  
Author(s):  
N T Thuan ◽  
M L Migueres ◽  
D Roche ◽  
G Roussel ◽  
G Mahuzier ◽  
...  
Keyword(s):  
Reversed Phase ◽  
Gas Liquid Chromatography ◽  
Tobacco Exposure ◽  
Coefficients Of Variation ◽  
Chromatographic Procedure ◽  
Phase Liquid ◽  
Liquid Chromatographic ◽  
Minimum Detectable Amount ◽  
Column Extraction

Abstract We report an analytical reversed-phase liquid-chromatographic procedure for quantifying nicotine and cotinine in urine, taking into account the presence of interfering caffeine frequently encountered in such specimens. These analytes are extracted from the alkalinized urine with chloroform. After evaporation of the chloroform, the residue is dissolved in methanol and injected into a chromatographic C18 column. Extraction recoveries averaged 80% to 97%. Chromatographic conditions were investigated to obviate caffeine interference. The proposed eluent mobile phase is a polar mixture of water, acetonitrile, methanol, and a pH 4 acetoacetate buffer (65/2/29/4 by vol) adjusted to pH 4.30 +/- 0.02 with triethylamine. High resolution and linearity were obtained for each analyte up to a concentration of 200 mg/L. The minimum detectable amount of each compound was 20 ng per injection, corresponding to 10 micrograms per liter of urine. Correlation with results of gas-liquid chromatography was excellent (r = 0.99). This simple, rapid procedure allows routine screening of tobacco exposure with acceptable precision: within- and between-run coefficients of variation were less than 2% and less than 5%, respectively.

scholarly journals Determination of Sulfonamides in Swine Meat by Immunoaffinity Chromatography

2000 ◽  
Vol 83 (4) ◽  
pp. 830-836 ◽  
Author(s):  
Jun Suo Li ◽  
Xi Wang Li ◽  
Jian Xiang Yuan ◽  
Xin Wang
Keyword(s):  
Liquid Chromatography ◽  
Reversed Phase ◽  
Immunoaffinity Chromatography ◽  
Uv Detection ◽  
Reversed Phase Liquid Chromatography ◽  
Specific Antibodies ◽  
Coefficients Of Variation ◽  
Phase Liquid ◽  
Immunoaffinity Columns

Abstract A procedure was developed for the preparation of anti-sulfonamide (SA) group-specific antibodies and immunosorbents. Sulfonamide haptens and conjugates were synthesized by building spacer arms on an N1 group of 4-aminobenzensulfonamide. The anti-SA group-specific antibodies and immunosorbents were prepared successfully. After extraction with methanol–water (8 + 2), sulfamonomethoxine, sulfadimethoxine, and sulfaquinoxaline were cleaned up on immunoaffinity columns and determined by reversed-phase liquid chromatography with UV detection at 270 nm. The recoveries from fortified swine meat (10–100 μg/kg) ranged from 70.8 to 94.1%, with coefficients of variation of 3.4–12.9%. Limits of detection were 1–2 μg/kg.

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