Study of the factors affecting the performance of microextraction by packed sorbent (MEPS) using liquid scintillation counter and liquid chromatography-tandem mass spectrometry

• Published in: Analytica chimica acta 2008-12, Vol.630 (2), p.116-123
• Main Authors: Altun, Zeki, Abdel-Rehim, Mohamed
• Format: Article
• Language: English
• Subjects: Analytical chemistry; Blood Chemical Analysis - instrumentation; Blood Chemical Analysis - methods; Bupivacaine - blood; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, High Pressure Liquid - methods; Exact sciences and technology; Liquid scintillation counter; Mass spectrometry; Microextraction by packed sorbent; Other chromatographic methods; Radioactively labelled bupivacaine; Radiochemical methods; Reproducibility of Results; Sample preparation; Scintillation Counting - methods; Sensitivity and Specificity; Solvents - chemistry; Spectrometric and optical methods; Syringes; Tandem Mass Spectrometry - methods
• ISSN: 0003-2670; 1873-4324
• DOI: 10.1016/j.aca.2008.09.067

Microextraction by packed sorbent (MEPS) is a new technique for sample preparation that can be connected on-line with LC or GC. In MEPS, approximately 1–2 mg of the solid packing material is inserted into a syringe (100–250 μL) as a plug. Sample preparation takes place on the packed bed. The bed can be packed or coated to provide selective and suitable sampling conditions. The new method is very promising for extraction of drugs and metabolites from biological samples. In this paper, some factors affecting the performance of MEPS such as recovery, carry-over, leakage, washing volume and elution volume were studied using C18 and hydroxylated polystyrene-divinylbenzene copolymer (ENV+) as sorbents. Radioactively labelled bupivacaine in plasma samples was used as test analyte. For the extraction of this drug, using methanol/water 95:5 (v/v) (0.25% ammonium hydroxide) was used as elution solvent. The analyte response increased with increasing the elution volume and it was linear upp up to 100 μL utilizing liquid scintillation counter. Further, for concentrating the sample, we found that MEPS may be used such that the sample can be drawn through the needle, up and down, several times. The analyte leakage increases as the volume washing increases, though higher washing volumes may also result in cleaner extracts. To eliminate analyte carry-over, the sorbents were washed first with 3 × 250 μL elution solution and then with 3 × 250 μL washing solution. In addition, the reproducibility measurements show relatively good relative standard deviation (RSD) % values concerning analyte recovery and analyte leakage. The present study provides an understanding of basic aspects when optimizing methods for MEPS. In this study, MEPS was used off-line with liquid scintillation counter and on-line with LC–MS/MS.