Pesticide trace analysis using solid-phase extraction and gas chromatography with electron-capture and tandem mass spectrometric detection in water samples

Abstract Background: Quantification of plasma free metanephrine (MN) and normetanephrine (NMN) is considered to be the most accurate test for the clinical chemical diagnosis of pheochromocytoma and follow-up of pheochromocytoma patients. Current methods involve laborious, time-consuming, offline sample preparation, coupled with relatively nonspecific detection. Our aim was to develop a rapid, sensitive, and highly selective automated method for plasma free MNs in the nanomole per liter range. Methods: We used online solid-phase extraction coupled with HPLC-tandem mass spectrometric detection (XLC-MS/MS). Fifty microliters plasma equivalent was prepurified by automated online solid-phase extraction, using weak cation exchange cartridges. Chromatographic separation of the analytes and deuterated analogs was achieved by hydrophilic interaction chromatography. Mass spectrometric detection was performed in the multiple reaction monitoring mode using a quadrupole tandem mass spectrometer in positive electrospray ionization mode. Results: Total run-time including sample cleanup was 8 min. Intra- and interassay analytical variation (CV) varied from 2.0% to 4.7% and 1.6% to 13.5%, respectively, whereas biological intra- and interday variation ranged from 9.4% to 45.0% and 8.4% to 23.2%. Linearity in the 0 to 20 nmol/L calibration range was excellent (R2 > 0.99). For all compounds, recoveries ranged from 74.5% to 99.6%, and detection limits were <0.10 nmol/L. Reference intervals for 120 healthy adults were 0.07 to 0.33 nmol/L (MN), 0.23 to 1.07 nmol/L (NMN), and <0.17 nmol/L (3-methoxytyramine). Conclusions: This automated high-throughput XLC-MS/MS method for the measurement of plasma free MNs is precise and linear, with short analysis time and low variable costs. The method is attractive for routine diagnosis of pheochromocytoma because of its high analytical sensitivity, the analytical power of MS/MS, and the high diagnostic accuracy of free MNs.

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Determination of fexofenadine in human plasma using 96-well solid phase extraction and HPLC with tandem mass spectrometric detection

Journal of Pharmaceutical and Biomedical Analysis ◽

10.1016/j.jpba.2004.02.016 ◽

2004 ◽

Vol 35 (4) ◽

pp. 837-846 ◽

Cited By ~ 29

Author(s):

I. Fu ◽

E.J. Woolf ◽

B.K. Matuszewski

Keyword(s):

Solid Phase Extraction ◽

Human Plasma ◽

Solid Phase ◽

Mass Spectrometric ◽

Mass Spectrometric Detection ◽

Tandem Mass ◽

Phase Extraction ◽

Tandem Mass Spectrometric

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Validation of an analytical method for the solid phase extraction, in cartridge derivatization and subsequent gas chromatographic–ion trap tandem mass spectrometric determination of 1-octen-3-one in wines at ngL−1 level

Analytica Chimica Acta ◽

10.1016/j.aca.2005.10.022 ◽

2006 ◽

Vol 563 (1-2) ◽

pp. 51-57 ◽

Cited By ~ 26

Author(s):

Laura Culleré ◽

Juan Cacho ◽

Vicente Ferreira

Keyword(s):

Solid Phase Extraction ◽

Analytical Method ◽

Ion Trap ◽

Solid Phase ◽

Mass Spectrometric ◽

Tandem Mass ◽

Phase Extraction ◽

Mass Spectrometric Determination ◽

Tandem Mass Spectrometric

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A sensitive and specific solid-phase extraction–gas chromatography–tandem mass spectrometry method for the determination of 11 haloacetic acids in aqueous samples

European Journal of Mass Spectrometry ◽

10.1177/1469066718781302 ◽

2018 ◽

Vol 24 (5) ◽

pp. 375-383 ◽

Cited By ~ 5

Author(s):

Aziz Kinani ◽

Jérôme Olivier ◽

Adrien Roumiguières ◽

Stéphane Bouchonnet ◽

Said Kinani

Keyword(s):

Mass Spectrometry ◽

Gas Chromatography ◽

Standard Deviation ◽

Solid Phase Extraction ◽

Water Samples ◽

Solid Phase ◽

Haloacetic Acids ◽

Tandem Mass ◽

Phase Extraction ◽

Relative Standard

A method for the analysis of 11 haloacetic acids in water samples has been developed. It involves enrichment of the target analytes from water samples by solid-phase extraction, derivatization to methyl esters, and gas chromatography coupled with tandem mass spectrometry determination. Gas chromatography conditions were optimized for a good separation of all haloacetic acids in a short runtime. Data were acquired in the multiple reaction monitoring mode. Six solid-phase extraction sorbents among the most widely used in environmental analysis were tested. Bakerbond SDB was retained because it has been shown to provide the best results for a large class of targeted haloacetic acids. The performances of the developed method have been assessed according to the French Standard NF T 90-210. The calibration curves for all the studied haloacetic acids had consistent slopes with r2 values > 0.99. Quantification limits between 0.01 and 0.50 µg l−1 were achieved. Satisfactory repeatability (relative standard deviation ≤ 14.3%) and intermediate precision (relative standard deviation ≤ 15.7%) were obtained. Applied to the analysis of 15 untreated water samples collected from three rivers, the method allowed the detection of five haloacetic acids including monochloroacetic acid (in 100% of the samples, <0.5–1.85 µg l−1), dichloroacetic acid (87%, <0.05–0.22 µg l−1), trichloroacetic acid (93%, <0.05–0.52 µg l−1), dibromoacetic acid (53%, <0.01–0.40 µg l−1), tribromoacetic acid (20%, <0.05–0.14 µg l−1), and bromodichloroacetic acid (6%, < 0.05 µg l−1).

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