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1

Using HPLC method with DAD detection for the simultaneous determination of 15 drugs in surface water and wastewater

100%

Baranowska I. , Kowalski B.

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nr 1

EN

Using HPLC method with DAD detection for the simultaneous determination of 15 pharmaceuticals from different therapeutic groups in surface water and wastewater was proposed. The determined drugs included the analgesic non-steroidal anti-inflammatory drugs (NSAIDs) paracetamol (PAR), metamizole (MTZ), aspirin (ASP), salicylic acid (SAL), ibuprofen (IBU), ketoprofen (KET), diclofenac (DIC), and naproxen (NAP); the corticosteroids dexamethasone (DEX) and prednisolone (PRE); the β-blockers carvedilol (CAR), metoprolol (MET), propranolol (PRO), and sotalol (SOT); and the anticonvulsant carbamazepine (CBM). Three solid-phase extraction (SPE) columns were examined for the pre-concentration of water samples: the Oasis HLB, NEXUS and Bond Elut ENV. The concentration level for which each method was validated in spiked water samples was 0.2 μg/L. The Oasis HLB column yielded the best recovery efficiency. Different HPLC columns were examined to achieve the best separations with the shortest possible time. The best column, C30 and was used for the determination of drugs from water samples.. The proposed method was applied to the analysis of water samples, mostly from rivers, and can be used for screening as a rapid and low-cost analytical tool. However, to confirm the positive findings MS techniques should be applied.

2

The determination of preservatives in cosmetics and environmental waters by HPLC

100%

Baranowska I. , Wojciechowska I.

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nr 6

EN

A method for the simultaneous determination of six preservatives in cosmetic and pharmaceutical products, as well as in surface waters, using high performance liquid chromatography (HPLC) has been developed. Methylisothiazolinone (MI), chloromethylisothiazolinone (CMI), benzyl alcohol (BA), potassium sorbate (PS), sodium benzoate (SB), and methylparaben (MP) were separated on a Develosil RP Aqueous AR-5 RP-30 (250 x 4.6 mm, 5.0 µm) column, using a gradient elution with acetonitrile and 0.1% aqueous solution of formic acid. Acetonitrile content is increased during the analysis from 15% to 25%. The analysis time was 22 minutes. The linearity ranges of calibration curves for the standards dissolved in methanol are: 1.83-18.33 µg/mL for MI, 2.50-25.00 µg/mL for CMI, 10.00-100.00 µg/mL for BA, 0.50-10.00 µg/mL for PS, and 1.00- 10.00 µg/mL for SB and MP. The linearity ranges of analytes for the water matrix are as follows: 3.17-18.33 µg/mL for MI, 3.50-25.00 µg/mL for CMI, 25.00-100.00 µg/mL for BA, 2.50-15.00 µg/mL for PS, and 2.50- 10.00 µg/mL for SB and MP. The limits of detection and quantification for the determined compounds are within the following ranges: LOD – 0.15-5.3 µg/mL and LOQ – 0.45-16 µg/mL. The quantitative extraction of analytes from solid samples and liquid samples with a high density and viscosity (cosmetics, pharmaceuticals) of the recoveries order 69-119% was performed using an ultrasoundassisted extraction with methanol. For the purpose of the analysis of environmental water samples, a method for extracting the analytes using solid-phase extraction technique (SPE) also was developed, allowing for the quantitative isolation of the analytes from water samples (recoveries of 65.4-105.6%) and for the 600-fold concentration. As a sorbent in SPE, cartridges with HLB filling were used (Oasis HLB, 6 mL, 500 mg). The method developed was applied to the analysis of the following samples: face tonics, creams, lotions, shower gels, face masks, and syrups for the content of determined preservatives, as well as for the detection and identification of its residues in surface waters. Four of the six chosen analytes were identified in the waters. The most detected and determined compound was SB (up to 3.12 µg/L). There are also detected and determined CMI (up to 11.57 µg/L), BA (up to 35.1 µg/L), and MP (in amounts higher than method detection limit but smaller than method quantification limit). The long-term stability of the compounds in surface waters also was determined. The stability of the determined compounds in environmental water varies, the most stable compounds are MI and BA, while the least stable are CMI and MP.

3

HPLC w analizie metalotionein

80%

Baranowska I. , Świerczek S. , Price R.

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tom z. 147

79-85

PL

Opracowano metodę HPLC do analizy metalotionein zawierających Pb i Cd. Aplikację metody przeprowadzono na próbkach moczu, po uprzednim wzbogaceniu metodą ekstrakcji do fazy stałej.

EN

HPLC methods for the analysis of metallotionein has been worked out. HPLC was used to detection, metalltionein in human's urine, after solid phase extraction.

4

Differential pulse polarography in the analysis of products from coal treatment

80%

Baranowska I. , Slaczka A. , Srogi K.

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nr 1

EN

The content of the heavy metals cadmium, zinc, nickel, lead and molybdenum in products and waste coming from fuel processing (originating from power plants and coal mines) was determined using DPV. Samples were digested in a microwave mineralizer in mixtures of HNO3 + HClO4 acids (3:2; 4:2 v/v). The following certified reference materials were used in these investigations: fly ash (CTA-FFA-1), apatite concentrate (CTA-AC-1) and coal (BCR-40).

5

Determination of metals in human placenta using graphite furnace atomic absorption spectroscopy

80%

Baranowska I. , Aleksandrowicz R. , Cekanski A. , Baranowski J.

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nr 1

EN

Lead, cadmium, zinc, manganese, chromium, cobalt, copper, and molybdenum concentrations were measured in 50 samples of placenta tissues. The samples came from Tychy in the Upper Silesian Industrial District (Poland), where the population is exposed to enormously increased levels of heavy metals. GFAAS technique was used. Various methods of ashing samples were examined. Wet ashing under pressure in the teflon bomb at 110°C with HNO, and wet ashing under normal pressure with HN03 + H202 are considered to be the best ones. Mean concentrations of metals in the placenta were determined. Coexistence of increased levels of various metals was checked. Concentration of heavy metals in the samples coming from the polluted industrial territory is higher than in those collected in cleaner regions.