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Scutellaria L. is a diverse genus of the Lamiaceae (Labiatae) family of over 300 herbaceous plants commonly known as skullcaps. Various species of Scutellaria are used as ethnobotanical herbs for the treatment of ailments like cancer, jaundice, cirrhosis, anxiety, and nervous disorders. Scutellaria incana L., commonly known as the Hoary skullcap, is a traditional medicinal plant used by native Americans as a sedative for nervousness or anxiety. S. incana metabolites were identified by comparing their high-performance liquid chromatography (HPLC) retention times and mass spectra with those of the corresponding authentic standards. Where standards were unavailable, the structures were characterized on the basis of their tandem mass spectrometry (MS/MS) spectra following collision-induced dissociation (CID) and the accurate masses of the corresponding deprotonated molecules [M-H] (mass accuracy ± 5 ppm). A total of 40 flavonoids, including two phenolic glycosides, were identified from leaves, stems, and roots of S. incana. Differences in the flavonoid composition between leaves, stems, and roots in S. incana were observed although the flavonoid profile of S. incana is consistent with other Scutellaria species. Further work should focus on assessing the potential of S. incana as a source of these bioactive metabolites.

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A simple, selective, and sensitive thin-layer chromatographic—densitometric method has been developed for the determination of sulfasalazine besides its possible impurities in pharmaceutical preparations. The mobile phase was composed of ethyl acetate—methanol—ammonia 25% 10:7:3 (υ/υ/υ), and the stationary phase was aluminum plates precoated with silica gel 60 F254 that enabled to obtain well resolved peaks of sulfasalazine and its impurities. The developed chromatograms were analyzed densitometrically at λ = 360 nm. R F values and ultraviolet (UV) spectra were used to identify the compounds. The developed method is highly sensitive (limit of detection [LOD] = 17.11 ng spot−1, limit of quantitation [LOQ] = 51.84 ng spot−1), precise (relative standard deviation [RSD] = 1.43%–4.28%), and accurate (RSD = 1.64%–4.27%). The linearity of the method was checked within the range 20–120 ng spot−1. The method was successfully applied for the determination of sulfasalazine in pharmaceutical preparations besides its impurities. The structures of impurities present in the standard substance and in pharmaceutical preparations were established by ultra-performance liquid chromatography—tandem mass spectrometry (UPLC—MS/MS) technique.

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Palmatine is a compound with good water solubility extracted from Coptis chinensis, Fibraurea recisa Pierre, Cortex Phellodendri Chinensis. Palmatine has good antibacterial activity and mainly used for the treatment of bacterial dysentery, gynecological inflammation, surgical infection, and conjunctivitis. It has anti-diabetic, anti-oxidant, and cognitive-enhancing activities. In this study, we used UPLC-MS/MS to determinate palmatine in rat plasma, and investigated its pharmacokinetics. Coptisine was utilized as an internal standard (IS), and acetonitrile precipitation method was used to process the plasma samples. Chromatographic separation was achieved using a UPLC BEH C18 column using mobile phase of acetonitrile- 0.1% formic acid with gradient elution. Electrospray ionization (ESI) tandem mass spectrometry in multiple reaction monitoring (MRM) mode with positive ionization was applied. The results indicated that within the range of 1–500 ng/mL, linearity of palmatine in rat plasma was acceptable (r > 0.995), and the lower limit of quantification (LLOQ) was 1 ng/mL. Intra-day and inter-day precision RSD of palmatine in rat plasma were less than 14%. Accuracy range was between 93.7 and 107.1%, and matrix effect was between 101.6 and 109.4%. The method was successfully applied in the pharmacokinetics of palmatine in rats after oral and intravenous administration. The absolute bioavailability of the palmatine was 15.5% in rats.

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The composition and concentration of natural products largely depend on a plant part, development stage, cultivar, and growing conditions. This study evaluated the influence of cultivars and production systems on the composition of natural products (benzoxazinoids) in wheat aerial parts. The determination of benzoxazinoids was performed by combining pressurized liquid extraction, ultra-performance liquid chromatography, and tandem mass spectrometry. Six benzoxazinoids were identified and quantitated in wheat varieties. Significant differences were observed among the examined varieties. The average concentrations of total researched compounds were definitely higher in the organically produced spring wheat cultivars than in the winter ones. The content of these compounds in the same varieties grown under organic and conventional systems showed their higher content under the organic one. The main benzoxazinoids detected in wheat varieties were 2,4-dihydroxy-7-methoxy-1,4-benzoxazin-3-one glucoside (DIMBOA-Glc) and 6-methoxy-2-benzoxazolinone (MBOA). The richest sources of benzoxazinoids were Brawura, Łagwa, and Kandela (52.46, 34.67, and 30.14 μg/g dry weight [DW], respectively).

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An improved ion-pairing reversed-phase high-performance liquid chromatography method coupled with evaporative light scattering detection (HPLC-ELSD) was developed to determine spectinomycin and its related substances in commercial samples. The method was validated in accordance with International Conference on Harmonization (ICH) guidelines. The specificity of the HPLC-ELSD method was similar to that of the European Pharmacopoeia (Ph. Eur.) method, and repeatability and robustness were markedly improved relative to other reported methods due to our empirical evaluation of separation columns. Indeed, it is a more specific assay of spectinomycin than traditional microbiological techniques. The HPLC-ELSD method was used to evaluate the impurity profiles of eight compounds in seven spectinomycin batches from five different companies. Liquid chromatography coupled with electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) was employed to characterize the structures of these compounds. Though the HPLC-ELSD method was not as sensitive as the Ph. Eur. method, its limit of quantitation (LOQ) (0.16%) was lower than the disregard limit (0.3%) described by the Ph. Eur. 7.0. This suggests that the HPLC-ELSD method is appropriate for routine analysis of spectinomycin and its related substances.

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A rapid method has been used for simultaneous identification of both hydrophilic and lipophilic compounds from Radix Salviae Miltiorrhizae (RSM, the root of Salvia miltiorrhiza BGE.) by ultra-performance liquid chromatography/quadrupole time-offlight mass spectrometry (UPLC/Q-TOF-MS). A total of 58 compounds extracted by methanol were detected and tentatively identified within 20 min, including hydrophilic phenolics, lipophilic diterpenoids, a verbascose, and several organic acids. These compounds were separated on an Acquity UPLC BEH C18 column and identified based on tandem mass spectrometry (MS/MS) fragmentation patterns under the positive and negative ion modes, respectively. Among them, micranthin B and 9-oxo-10E,12Zoctadecadienoic acid were reported in RSM for the first time. Their fragmentation patterns in electrospray ionization (ESI)—MS/MS spectra were first investigated by matching their accurate molecular masses. This contribution presented one of the first reports on the analysis of hydrophilic phenolics and lipophilic diterpenoids from Radix Salviae Miltiorrhizae using UPLC/Q-TOF-MS. The results demonstrated that UPLC/Q-TOF-MS method could be applied to rapidly and expediently describe and provide comprehensive chemical information for simultaneous analysis of two different polar components in RSM.

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The effect of free-range versus cage management system on corticosterone transfer into the eggs was studied in laying hens. Hungarian Yellow laying hens (age: 21 weeks, body weight: 2.0 ± 0.5 kg) were divided into two groups in the spring: Group I, free-range keeping (n = 15 layers, density: ≯ 0.5 bird/m2) in outdoor runs, with continuous access to a commercial layer feed; Group II, hens kept in battery cages (n = 17 layers, density: 2 birds/m2, natural light, continuous access to feed and water). Eggs were collected after a one-week adaptation period on days 2, 7 and 16. Corticosterone (CST) was extracted from homogenised egg samples using an ASE-200 Accelerated Solvent Extractor and then assayed by liquid chromatography linked with tandem mass spectrometry (LC-MS/MS) [Thermo Quest Surveyor high-performance liquid chromatography (HPLC) interfaced via Atmospheric Pressure Chemical Ionisation (APCI) ion source to Finnigan/Thermo Quest LCQ Deca MS/MS] using dexamethasone as internal standard with positive APCI ionisation. CST concentrations of whole eggs laid by free-range hens on days 2, 7 and 16 were 0.370 ± 0.218, 0.259 ± 0.066 and 0.915 ± 0.745 ng·g-1, respectively, while those of eggs laid by caged hens were 0.206 ± 0.157, 0.223 ± 0.165 and 0.184 ± 0.110 ng·g-1 at the above sampling times. It is concluded that in free-range laying hens the sharp changes of environmental weather conditions significantly increased the corticosterone content of eggs, while the environmentally controlled and closed battery cage management technology resulted in relatively uniform corticosterone concentrations in the whole eggs.

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A simple and sensitive liquid chromatography—tandem mass spectrometry method was developed for the quantification of atorvastatin, ortho-hydroxyatorvastatin, para-hydroxyatorvastatin, and atorvastatin lactone in rat plasma. Solid-phase extraction was used for preparation of samples. Rosuvastatin was chosen as an internal standard. Chromatographic separation was achieved on ZORBAX Eclipse C18 Analytical, 4.6 × 100 mm (3.5 μm) column with a gradient mobile phase composed of acetonitrile and 0.1% acetic acid, at a flow rate of 400 μL min−1. The column was kept at constant temperature (25 °C), and autosampler tray temperature was set at 4 °C. The following selected reaction monitoring (SRM) transitions were selected: (m/z, Q1 → Q3, collision energy) atorvastatin (559.47 → 440.03, 22 eV), atorvastatin lactone (541.36 → 448.02, 19 eV), ortho-ohydroxyatorvastatin (575.20 → 440.18, 20 eV), para-hydroxyatorvastatin (575.54 → 440.18, 20 eV), and rosuvastatin (482.25 with selected combination of two fragments 257.77, 31 eV, and 299.81, 35 eV) in positive ion mode. The method was validated over a concentration range of 0.5–20 ng mL−1 for ortho-hydroxyatorvastatin and para-hydroxyatorvastatin and 0.1–20 ng mL−1 for atorvastatin and atorvastatin lactone with excellent linearity (r 2 ≥ 0.99). This method demonstrated acceptable precision and accuracy at four quality control concentration levels. The detection limits were 0.1 and 0.13 ng mL−1 for orth-ohydroxyatorvastatin and para-hydroxyatorvastatin, respectively, and 0.05 ng mL−1 for atorvastatin and atorvastatin lactone. All analytes were found to be stable at examined conditions. Validated method was applied for determination of atorvastatin and its metabolites in plasma of experimental animals.

Open access

Aegle marmelos Correa (Bael tree) is a medicinal fruit tree, widely used for healing purposes in various systems of medicines. Coumarins and alkaloids present in various parts of bael tree including roots and fruit pulp are the primary active constituents implicated for its biological activities. An efficient liquid chromatography–electrospray ionization—tandem mass spectrometry (LC—ESI—MS/MS) method was developed for identification and simultaneous determination of four coumarin derivatives, namely, umbelliferone, psoralene, marmin, and imperatorin, and an alkaloid, skimmianine, in root and stem bark of A. marmelos. The chromatographic separation of analytes was performed on Altima C18 (50 × 4.6 mm, 3 μm) column using methanol and 0.1% acetic acid in water (54:46, v/v) as the mobile phase under isocratic conditions. The LC–MS/MS parameters were optimized in the positive ionization mode using electrospray ionization source. The quantification of the analytes was performed using multiple reaction monitoring (MRM) transitions, umbelliferone (m/z 163.1 → 107.1), psoralene (m/z 187.2 → 131.1), marmin (m/z 333.5 → 163.2), imperatorin (m/z 271.1 → 203.1), and skimmianine (m/z 260.1 → 227.0). The extraction method was standardized for optimum yield of coumarin derivatives and the alkaloid in different extraction solvents. Higher yield of the analytes was found in methanolic extracts in comparisons to petroleum ether, chloroform, ethyl acetate, ethanol, and water. The method was validated for linear range, intra- and inter-batch precision and accuracy. The distribution of coumarin derivatives and an alkaloid was found to vary significantly in different plant samples, and their concentration was much higher in roots as compared to stem bark.

Open access
Acta Chromatographica
Authors: Biljana K. Tubić, Bojan D. Marković, Sandra S. Vladimirov, Slavica M. Ristić, Branka M. Ivković, Miroslav M. Savić, Jelena M. Poljarević, and Tibor J. Sabo

A series of new (S,S)-ethylenediamine-N,N′-di-2-(3-cyclohexyl)propanoate esters has shown cytotoxic activity towards human leukemic cell lines. The aim of this study was to develop and validate a bioanalytical method for quantification of (S,S)-O,O-diethyl-ethylenediamine-N,N′-di-2-(3-cyclohexyl)propanoate dihydrochlorides (DE-EDCP) and its metabolite, substituted propanoic acid (EDCP), in mouse serum by ultra high-performance liquid chromatography—tandem mass spectrometry (UHPLC—MS/MS). Structural analog, derivative of 1,3-propanediamine, was used as an internal standard (IS). Sample preparation employed protein precipitation by acetonitrile and subsequent centrifugation. Optimal UHPLC separation conditions were set to achieve simultaneous determination of both compounds in a short run time of 6 min. Additionally, the selected reaction monitoring (SRM) mode developed in this method allowed a highly sensitive, accurate, and precise identification of compounds of interest. The lower limit of quantitation (LOQ) was 1.3 ng mL−1 for DE-EDCP and 0.3 μg mL−1 for EDCP. The calibration curves were linear over the concentration range of 1.3–26.7 ng mL−1 and 0.3–6.7 μg mL−1 for DE-EDCP and EDCP, respectively. Precision (%CV) and accuracy (%RE) for DE-EDCP and EDCP ranged from 3.5% to 16.0% and from 1.8% to 14.4%, respectively.

The validation process was performed in accordance with the regulatory guidance/guideline, and all of the obtained results met the established acceptance criteria. The newly developed and validated UHPLC—MS/MS method is rapid, sensitive, and selective, and it can be successfully applied to drug monitoring in nonclinical studies.

Open access