Comparison between thin-layer chromatography and overpressured layer chromatography fingerprints of commercial essential oils and accelerated solvent extraction plant extracts

Developing fit-to-purpose analytical screening methods for plant marker constituents by simple and affordable techniques represents a constant and important request from the current transformation chain of plant products. In this work, methods developed on classical thin-layer chromatography (TLC) and overpressured layer chromatography (OPLC) have been applied on some of the most valuable commercial plant products, such as star anise (Illicium verum Hook. f.) essential oil and extracts, common thyme (Thymus vulgaris L.) and sweet fennel (Foeniculum vulgare Mill.) essential oils and acerola fruit (Malpighia punicifolia L.) hydroalcoholic extracts, to evaluate OPLC potentiality in comparison with TLC performances in the detection of some characteristic constituents. OPLC provided higher performance with respect to TLC in all experiments performed due to higher selectivity demonstrated on all the tested marker compounds except for flavonoids in acerola extracts. Considering the usage of planar chromatography in the quality control of plant derivatives, the present paper shows how the OPLC protocols were both highly time- and solvent-saving in comparison with classical TLC.

     

Fully automated solid-phase microextraction-fast gas chromatography-mass spectrometry method using a new ionic liquid column for high-throughput analysis of sarcosine and N-ethylglycine in human urine and urinary sediments

A fully automated, non invasive, rapid and high-throughput method for the direct determination of sarcosine and N-ethylglycine in urine and urinary sediments using hexyl chloroformate derivatization followed by direct immersion solid-phase micro extraction and fast gas chromatography-mass spectrometric analysis was developed and validated. The use of a new ionic liquid narrow bore column, as well as the automation and miniaturization of the preparation procedure by a customized configuration of the utilized XYZ robotic system, allowed a friendly use of the GC apparatus achieving a quantitation limit of 0.06 μg L(-1) for sarcosine, good repeatability with CV always lower than 7% and reduced analysis times useful for point-of-care testing. The method was then applied for the analysis of 56 samples of urine and urinary sediments in healthy subjects, in those with benign prostatic hypertrophy and in patients with clinically localized prostate cancer. The results obtained showed that the medians of sarcosine/creatinine in urine were 103, 137 and 267 μg g(-1) respectively, thus assessing the potential use of sarcosine as urinary biomarker for prostate cancer detection. The highest values of sensitivity (79%) and specificity (87%) were obtained in correspondence of a cut-off value of 179 μg sarcosine(g creatinine)(-1), thus by using this cut-off threshold, sarcosine was significantly associated with the presence of cancer (p<0.0001). Finally, ROC analyses proved that the discrimination between clinically localized prostate cancer and patients without evidence of tumor is significantly correlated with sarcosine.