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Simultaneous quantification of five lignans from Schisandra chinensis in various tissues of rats

Su Lian-Lin, Cheng Xue, Ding Xi-Yan, Mao Chun-Qin, Lu Tu-Lin, Hao Min, Li B.-W., Qin Sirui

Acta Chromatographica

2019

Vol. 31, no. 2

113--119

In this research study, a rapid, sensitive, and specific high-performance liquid chromatography–electrospray ionization–tandem mass spectrometry (HPLC–ESI–MS/MS) method was established and validated, in regard to the simultaneous quantification of five sedative and hypnotic lignans (schisandrin, schisandrol B, schisantherin A, deoxyschisandrin, and schisandrin B) in various tissues of rats (including heart, liver, spleen, lung, and kidney). The purpose of the study was to clarify the tissue distribution of the total lignans extract of Schisandra chinensis (SC). Then, the analytes were separated on a MERCK Purospher STAR LP C18 column (250 mm × 4.6 mm, 5 μm), with a mobile phase consisting of 0.05% (v/v) formic acid acetonitrile, and 0.05% (v/v) formic acid water, and a flow rate of 1 mL/min. All of the calibration curves of the five components showed good linearity (r > 0.9950), with ranges of 4.8 to 1920 ng/mL for analytes. The intra-day and inter-day precisions (relative standard deviation [RSD] %) were within 13.76% for all of the analytes. The average recoveries of the five analytes were greater than 85.23%, and the mean value of the matrix effect ranged from 82.3% to 93.4%. The five analytes were confirmed to be stable during the storage, preparation, and analytic procedures. The major target tissues of the total lignans extract of the SC in the rats were the livers and kidneys.

Validation and application of HPLC–ESI–MS/MS method for the determination of irsogladine

Hoang N. H., Huong N. L., Hong S.-Y., Park J.-W

Acta Chromatographica

2017

Vol. 29, no. 4

459--462

A highly sensitive analytical tool for the fast quantification of irsogladine in human plasma was developed. Cleanup using a solid-phase extraction technique is a simple method for extracting both irsogladine and lamotrigine (internal standard) spiked into human plasma. The resolvable separation of both analytes through reversed-phase high-performance liquid chromatography (HPLC) was carried out within 5 min. The HPLC–electrospray ionization (ESI)–tandem mass spectrometry (MS/MS) method, which was operated in a selected reaction monitoring mode specific to the target analytes, was verified for use in the quantification of irsogladine. The inter- and intra-day precision (relative standard deviation, RSD) of irsogladine spiked into quality control samples were <7%, and their accuracies were between 96.6% and 102.1%. The calibration curve for irsogladine spiked into human plasma was linear over the range from 1.8 to 100 ng mL−1 with lower limit of quantification at 1.8 ng Ml-1. The established method was successfully applied for a bioequivalence study of irsogladine.

Occurrence of acidic pharmaceuticals in the Warta River in Poland

Kasprzyk-Hordern B., Dąbrowska A., Vieno N., Kronberg L., Nawrocki J.

Chemia Analityczna

2008

Vol. 53, No. 2

289-303

The occurrence of five acidic pharmaceuticals (ibuprofen, naproxen, ketoprofen, diclofenac, bezafibrate and clofibric acid) in the Warta River in Poland has been discussed. A significant effect of the effluents of Wastewater Treatment Plants (WWTPs) on the quality of recipient water has been shown. Diclofenac, ibuprofen, naproxen, and ketoprofen were found in all samples collected along the Warta River at average concentrations of several ng L-1'. Average concentration of the above pharmaceuticals in raw sewage entering wastewater plants was at the level of a few μg L-1. The efficiency of pharmaceuticals' removalfrom the raw sewage was very high and reached 97-100%. Diclofenac was the only compound, which exhibited a significant resistance towards the treatment (< 65%), and accordingly its concentration in the recipient water was the highest. Solid phase extraction (SPE) was use for separation of pharmaceuticals from the water phase and HPLC-ESI-MS/MS system was applied for the analysis.

W pracy przedstawiono wyniki badań nad obecnością w rzece Warcie pięciu farmaceutyków o charakterze kwasowym: ibuprofenu, naproksenu, diklofenaku, bezafibratu i kwasu klofi-browego. Związki te dostają się do środowiska najczęściej wraaze ściekami komunalnymi, ponieważ część z nich odporna na procesy biodegradacji nie ulega całkowitej eliminacji w trakcie procesów oczyszczania. Diklofenak, ibuprofen, naproksen i ketoprofen wykryto we wszystkich próbkach wody średnio na poziomie ng L-1. Średnie stężenie powyższych farmaceutyków w nieoczyszczonej wodzie przed oczyszczalniami było na poziomie kilku μL-1. Skuteczność usuwani a badanych farmaceutyków w oczyszczalni ścieków wynosiła około 97-100%, jedynie w przypadku diklofenaku była niższa niż 65%. W pracy zastosowano technikę SPE do ekstrakcji i zatężania próbek oraz układ analityczny HPLC-ESI- MS/MS.