Non-equilibrium solid-phase microextraction coupled directly to ion-trap mass spectrometry for rapid analysis of biological samples

Hout, M.W.J van; Jas, V.; Niederländer, H.A.G.; Zeeuw, Rokus A. de; Jong, Gerhardus J. de

doi:10.1039/b110729a

Cited by 16 publications

(18 citation statements)

References 27 publications

(61 reference statements)

Supporting

Mentioning

Contrasting

Order By: Relevance

“…A limit of quantitation (LOQ; RSD a 15%) of about 1 ng/mL could be obtained. The results show a slight improvement of the reproducibility in comparison with our previous study [14], in which rapid nonequilibrium SPME at room temperature was applied (intraday and interday RSD lower than 14%). From LOD to maximum concentration studied.…”

Section: Applicationmentioning

confidence: 37%

“…In a previous study by our group [14] the model compound lidocaine was determined in urine by SPME directly coupled to MS, thus eliminating the separation step and showing the suitability of SPME for determination of less volatile compounds after liquid desorption. Good selectivity was obtained by the SPME procedure and by the use of MS/MS.…”

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Ultra‐rapid non‐equilibrium solid‐phase microextraction at elevated temperatures and direct coupling to mass spectrometry for the analysis of lidocaine in urine

Hout¹,

Jas

Niederländer

et al. 2003

J of Separation Science

View full text Add to dashboard Cite

Ultra-rapid non-equilibrium solid-phase microextraction at elevated temperatures and direct coupling to mass spectrometry for the analysis of lidocaine in urine Solid-phase microextraction (SPME) has been directly coupled to an ion-trap mass spectrometer (MS) for the determination of the model compound lidocaine in urine, hereby applying MS/MS [fragmentation of [M + H] + (m/z 235) to a fragment with m/z 86]. The throughput of samples has been increased using non-equilibrium SPME with polydimethylsiloxane (PDMS) fibers. The effect of temperature on the sorption and the desorption was studied. Elevated temperatures during sorption (658C) and desorption (558C) had a considerable influence on the speed of the extraction. The desorption was carried out with a home-made desorption chamber allowing thermostating. Only 1 min sorption and 1 min desorption were performed, after which MS detection took place, resulting in a total analysis time of 3 min. Detection limits below 1 ng/ mL could be obtained despite yields of only 2.1 and 1.5% for a 100-and a 30-lm PDMS-coated fiber, respectively. Furthermore, the determination of lidocaine in urine had acceptable reproducibilities, i.e., relative standard deviations (RSDs) below 10%. A limit of quantitation (RSD a 15%) of about 1 ng/mL was obtained. No extra wash step of the extraction fiber was required after desorption if a 30-lm coating was used, whereas not all the analyte was desorbed from the 100-lm coating in a single desorption. Therefore, the SPME-MS/MS system with a 30-lm PDMS-coated fiber for rapid non-equilibrium SPME at elevated temperatures has interesting potential for highthroughput analysis of biological samples.

show abstract

Section: Applicationmentioning

confidence: 37%

Section: Introductionmentioning

confidence: 99%

Ultra‐rapid non‐equilibrium solid‐phase microextraction at elevated temperatures and direct coupling to mass spectrometry for the analysis of lidocaine in urine

Hout¹,

Jas

Niederländer

et al. 2003

J of Separation Science

View full text Add to dashboard Cite

show abstract

“…Detection limits were slightly higher in the second, although fewer interfering substances were observed. Lidocaine was also the object of an analytical investigation by van Hout et al [52]. In this work the SPME-HPLC interface was coupled directly to an atmospheric pressure chemical ionization (APCI)-MS/ ion trap for rapid analysis of the drug in urine samples.…”

Section: Biological Samplesmentioning

confidence: 99%

Coupling solid-phase microextraction to liquid chromatography. A review

Zambonin

2003

Anal Bioanal Chem

View full text Add to dashboard Cite

Solid-phase microextraction (SPME) is a technique for extraction of organic compounds from gaseous, aqueous, and solid matrices. SPME is rapid and simple, ideal for automation and for in situ measurements, and no harmful solvents are needed. The principle of SPME involves equilibration of the analytes between the sample matrix and an organic polymeric phase coated on a fused-silica fiber. SPME is traditionally combined with analysis by gas chromatography (GC) and this combination has proved sensitive, accurate, and precise for quantitative analysis of different classes of volatile compound. More recently SPME has been coupled with liquid chromatography to widen its range of application to non-volatile and thermally unstable compounds also. This article reviews the status of SPME coupled with liquid chromatography. It focuses on different applications of the technique, e.g. environmental samples, biological fluids, and food samples, to show that SPME-HPLC has great potential in the analysis of a wide range of compounds in different matrices.

show abstract

“…A first attempt to couple SPME with APCI-MS was made using a fibre coated with 100-1xm polydimethylsiloxane (PDMS) by which lidocaine was extracted from urine [2]. Urine was diluted with buffer pH 10 (1:1 v/v) prior to analysis.…”

Section: Extended Abstractmentioning

confidence: 99%

“…

High-throughput analysis of biological samples is becoming increasingly important. Good linearity (R > 0.99) was observed over the range 10 250 ngmL 1.A first attempt to couple SPME with APCI-MS was made using a fibre coated with 100-1xm polydimethylsiloxane (PDMS) by which lidocaine was extracted from urine [2]. In order to increase the speed even more, solid-phase extraction (SPE) and solid-phase microextraction (SPME) have been directly coupled to an ion-trap mass spectrometer (ITMS).

…”

mentioning

confidence: 99%

High-throughput analysis of biological samples by direct coupling of solid-phase (micro-)extraction and mass spectrometry

et al. 2002

Self Cite

View full text Add to dashboard Cite

High-throughput analysis of biological samples is becoming increasingly important. On-line sample pretreatment and separation increases the speed and reliability of the analysis. In order to increase the speed even more, solid-phase extraction (SPE) and solid-phase microextraction (SPME) have been directly coupled to an ion-trap mass spectrometer (ITMS). As a result, analysis times can be reduced to a few minutes.If SPE is directly coupled to the ITMS it is very important to obtain clean extracts to prevent detection problems, e.g. ion suppression. With a non-selective stationary phase, the removal of interfering matrix compounds requires an efficient washing step in which no elution of the analyte occurs. The choice of single MS vs. multiple-stage MS is also dependent on this step. Special attention has been paid to differences in chromatograms of blank samples and to ion-suppression effects. Extended AbstractMultiple-stage MS is very interesting for a reduction of matrix effects, and so a considerable increase of selectivity and sensitivity was obtained. Multiple-stage MS cannot eliminate ion suppression. SPE-MS methods with atmospheric pressure chemical ionisation (APCI) have been developed for the determination of clenbuterol in urine [1] and prednisolone in serum using a polydivinylbenzene (PDVB) and C18 stationary phase, respectively.A PDVB cartridge (10 • 2mm i. d.) allowed effective washing of the SPE phase, i.e. 50% (v/v) methanol could be used without elution of clenbuterol from the cartridge. This resulted in relatively clean extracts. Elution was performed with a flow-rate of 1.0mLmin 1 using a methanol gradient (50 to 70% in 2.5 min). However, for sensitive analysis MS-MS had to be applied. Consequently, a detection limit (LOD) of about0.5 ngmL 1 was observed for clenbuterol in urine. Despite the washing procedure severe ion suppression (45%) was observed for low levels of clenbuterol (0.5 10ngmL 1), whereas the ion suppression was less prominent for higher concentrations of clenbuterol (suppression about 4%). Even though the suppression was concentration dependent, good linearity was observed (R>0.99, range 1.0 250ngmL 1). The total analysis time was about 8.5 min, which is still relatively long due to rather low flow-rates that were applied during the different SPE steps.Prednisolone was extracted from serum by a C18 stationary phase (10 • 2 mm i.d.). Due to the apolar ring structure of the analyte it was possible to wash the stationary phase with 25% (v/v) methanol. Elution was performed using a methanol gradient (25 to 50% in 1.5 min with a 1-mL min 1 flow-rate). Subsequently, MS-MS was used for the analyis. The total set-up resulted in an LOD of 10 ng mL 1 of prednisolone in serum (Figure 1). The relatively high LOD is due to MS fragmentation of prednisolone. The total analysis time including sample pretreatment is about 5 min. No ion suppression was observed during the determination of prednisolone. Good linearity (R > 0.99) was observed over the range 10 250 ngmL 1.A first attempt to couple SP...

show abstract

Non-equilibrium solid-phase microextraction coupled directly to ion-trap mass spectrometry for rapid analysis of biological samples

Cited by 16 publications

References 27 publications

Ultra‐rapid non‐equilibrium solid‐phase microextraction at elevated temperatures and direct coupling to mass spectrometry for the analysis of lidocaine in urine

Ultra‐rapid non‐equilibrium solid‐phase microextraction at elevated temperatures and direct coupling to mass spectrometry for the analysis of lidocaine in urine

Coupling solid-phase microextraction to liquid chromatography. A review

High-throughput analysis of biological samples by direct coupling of solid-phase (micro-)extraction and mass spectrometry

Contact Info

Product

Resources

About