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UPLC-DAD determination of taxodione content in hairy roots of Salvia austriaca Jacq.

Kuźma Ł., Wysokińska H.

Acta Chromatographica

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2014

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Vol. 26, no. 4

671--681

EN

Taxodione is the abietane diterpenoid, which has been earlier reported to show cytotoxic, antitumor, antibacterial, and antioxidant properties. This compound has been isolated from a genetically transformed root culture of Salvia austriaca. However, no method for taxodione quantification is yet available. A validated ultra-performance liquid chromatography-diode array detector (UPLC-DAD) method was developed for the quantification of taxodione in a hexane extract taken from genetically transformed roots of S. austriaca. The developed UPLC-DAD method demonstrated good linearity in the range 10–500 μg mL−1 (r2 = 0.99988), high precision (relative standard deviation (RSD) <1.42%), and good repeatability (RSD <1.84%). The limits of detection and quantification of taxodione were found to be 0.48 ng and 1.60 ng, respectively. The recovery of taxodione ranged between 90.4 and 113.1%, and the RSD was less than 2.5%.The developed UPLC-DAD method was then used to determine the content of taxodione in various hairy root lines and changes in amount of the compound during the 50-day growth cycle of the culture. The content of taxodione in hairy root cultures of S. austriaca ranged from 0.29 to 1.12 mg g−1 dry weight depending on root line and stage of growth.

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Identyfikacja diuretyków w moczu techniką ultrasprawnej chromatografii cieczowej połączonej z tandemową spektrometrią mas (UPLC/MS/MS)

Tszyrsznic W., Stańczyk D., Pokrywka A., Kwiatkowska D.

Wiadomości Chemiczne

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2010

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[Z] 64, 3-4

319-333

EN

Diuretics are medicines that intensify the diuresis process. There are several types of diuretics (high ceiling loop diuretics, thiazides, calcium-sparing diuretics, potassium-sparing diuretics, osmotic diuretics). Generally all of them increase excretion of water from a body. According to the Prohibited List published by the World Anti-Doping Agency diuretics make a group of substances which is prohibited in sport at all times (in- and out-of-competition). This review describes shortly an ultra performance liquid chromatography technique, chemical properties of diuretics named in the WADA Prohibited List as well as a developed analytical method with the use of UPLC/MS/MS technique for determination of diuretics and other doping agents (stimulants, masking agents) in urine samples in comparison with a GC/MS method used earlier. Detailed extraction procedure and comparison of application of several organic solvents during extraction process were given. Parameters of MS/MS method have also been given. The described method was validated in accordance with EURACHEM "The Fitness for Purpose of Analytical Methods: A Laboratory Guide to Method Validation and Related Topics". Limits of detection and recovery level for all compounds in the method were evaluated. The developed method allows to detect most of diuretics at the levels of 1/5 MRPL (Minimum Required Performance Limits) and fulfills all requirements of the World Anti-Doping Agency.

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Development and validation of a stability-indicating UHPLC method for assay of felbamate and related substances

Shetty S. K, Surendranath K. V, Kaja R. K., Satish J, Jogul J, Manitripathi U

Acta Chromatographica

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2010

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Vol. 22, no. 2

161--172

EN

A new, sensitive, stability-indicating, and cost and time-effective isocratic reversed-phase UHPLC method has been developed for quantitative analysis of felbamate, an antiepileptic drug, both in the bulk drug and in pharmaceutical dosage forms. Chromatographic separation of felbamate and its two impurities was achieved on a C 18 column with a simple buffer-methanol mobile phase; the run time was 8 min. Quantification was achieved by ultraviolet detection. Resolution between the impurities was >2.0. Response was a linear function of concentration over the range 0.1–3.0 μg mL -1, correlation coefficient >0.999, for felbamate and the impurities. The method is capable of detecting the two impurities at levels of 0.002% (0.02 μg mL -1) of the test concentration of 1.0 mg mL -1 (1 μL injection). The same sensitivity was achieved for all the degradation products formed during stress studies in which the drug was subjected to hydrolysis, oxidation, photolysis, and thermal degradation. Substantial degradation occurred under acidic and basic conditions. The stressed test solutions were assayed against felbamate working standard and the mass balance in each case was close to 100%, indicating the method is stability-indicating. The method was validated for linearity, accuracy, precision, and robustness in accordance with ICH Guidelines.