Automated multi-dimensional liquid chromatography: sample preparation and identification of peptides from human blood filtrate

Abstract Solanesol, a naturally occurring constituent of tobacco, has been utilized as a good marker for environmental tobacco smoke particulate and as a noninvasive predictor of mainstream cigarette smoke tar and nicotine intake under naturalistic smoking conditions. A fast and accurate method for measuring free solanesol to assess tobacco smoke exposure is highly desirable. We have developed and validated a new environmentally friendly, high-throughput method for measuring solanesol content in discarded cigarette filter butts. The solanesol deposited in the used filters can be correlated with mainstream smoke deliveries of nicotine and total particle matter to estimate constituent delivery to smokers. A portion of filter material is removed from cigarette butts after machine smoking, spiked with internal standard solution, extracted and quantitatively analyzed using reverse-phase liquid chromatography coupled to a triple-quadrupole mass spectrometer. The new method incorporates a 48-well plate format for automated sample preparation that reduces sample preparation time and solvent use and increases sample throughput 10-fold compared to our previous method. Accuracy and precision were evaluated by spiking known amounts of solanesol on both clean and smoked cigarette butts. Recoveries exceeded 93% at both low and high spiking levels. Linear solanesol calibration curves ranged from 1.9 to 367 µg/butt with a 0.05 µg/butt limit of detection.

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Sample preparation procedure for determination of dopamine sulfate isomers in human urine by high-performance liquid chromatography with dual-electrode electrochemical detection

Journal of Chromatography B Biomedical Sciences and Applications ◽

10.1016/s0378-4347(00)83590-2 ◽

1986 ◽

Vol 381 ◽

pp. 241-248 ◽

Cited By ~ 10

Author(s):

Patrick G. Swann ◽

Mary Ann Elchisak

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Sample Preparation ◽

Electrochemical Detection ◽

Human Urine ◽

High Performance ◽

Preparation Procedure ◽

Sample Preparation Procedure

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Developments in mycotoxin analysis: an update for 2012-2013

World Mycotoxin Journal ◽

10.3920/wmj2013.1637 ◽

2014 ◽

Vol 7 (1) ◽

pp. 3-33 ◽

Cited By ~ 52

Author(s):

F. Berthiller ◽

P.A. Burdaspal ◽

C. Crews ◽

M.H. Iha ◽

R. Krska ◽

...

Keyword(s):

Mass Spectrometry ◽

Liquid Chromatography ◽

Sample Preparation ◽

Ergot Alkaloids ◽

Tandem Mass ◽

Wide Range ◽

Rapid Spread ◽

Food And Feed ◽

Mycotoxin Analysis ◽

The Individual

This review highlights developments in mycotoxin analysis and sampling over a period between mid-2012 and mid-2013. It covers the major mycotoxins: aflatoxins, Alternaria toxins, ergot alkaloids, fumonisins, ochratoxins, patulin, trichothecenes and zearalenone. A wide range of analytical methods for mycotoxin determination in food and feed were developed last year, in particular immunochemical methods and liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS)-based methods. After a section on sampling and sample preparation, due to the rapid spread and developments in the field of LC-MS/MS multimycotoxin methods, a separate section has been devoted to this area of research. It is followed by a section on mycotoxins in botanicals and spices, before continuing with the format of previous reviews in this series with dedicated sections on method developments for the individual mycotoxins.

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