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1

Identification and Correlation Test of Mercury Levels in Community Urine at Traditional Gold Processing Locations

Lensoni, Adlim M., Kamil Hajjul, Karma Taufiq, Suhendrayatna

Journal of Ecological Engineering

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2023

|

Vol. 24, nr 3

357--365

EN

Gold processing activities in Paya Seumantok Village, Krueng Sabee District, Aceh Jaya Regency, are known to utilize traditional mercury, posing a health threat to the workers and the local community. This study aims to identify local people’s urinary mercury levels near the gold processing plant in Paya Seumantok Village and to see the relationship between mercury levels and disease symptoms exhibited by the local people. To this end, ninety-one participants were recruited from a total member of a population of 928 people, determined using Slovin’s formula. The urine sample was collected using a purposive sampling technique following the procedure set by the regulation of the Minister of Health no. 43/2013. AAS Instrument was used to analyze the urinary mercury level. Sixteen out of 91 urine samples exhibited no mercury, while the rest, 75 samples, were found to contain mercury. The average urinary mercury level among local people near the site was 8.392 μg/L (SD: 6.721 g/L), while the minimum and maximum urinary mercury levels in this study were 0.19 μg/L and. 28.31 μg/L, respectively. Thirty-six samples were found to have mercury levels exceeding the acceptable threshold (7 μg/L), while thirty-nine samples had urinary mercury levels below the threshold. This study concluded that there is no relationship between urinary mercury levels and symptoms of acute and chronic diseases experienced local community and workers at the gold processing site in Paya Seumantok Village, Krueng Sabee District, Aceh Jaya Regency (p > 0.05).

2

Rapid measurement of anticoagulant rodenticides in human blood and urine using online turbulent flow chromatography coupled with liquid chromatography–tandem mass spectrometry

Fang Li, Qiu Fengmei, Yu Xinwei, Yan Jianbo, Zhu Yanhua

Acta Chromatographica

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2021

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Vol. 33, no. 4

361--370

EN

Anticoagulant rodenticides (ARs) are widely used to control rodents. A method based on online turbulent flow chromatography (TFC) combined with LC-MS/MS has been established for rapid quantitative determination of eight ARs in human blood and urine. This method, which does not require time-consuming pre-processing steps, renders it especially suited for use in emergency poisoning cases. Sample preparation, including extraction, centrifugation, and filtration, was followed by online clean-up using TFC. The total run-time was within 13.5 min, including online purification, chromatographic separation, and re-equilibration of the TFC system. The parameters for sample extraction, purification, separation, and detection in this study were optimized separately. The linear regression coefficients of matrix-matched calibration standard curves established for quantification were greater than 0.9976. The limit of quantification (LOQ) for the method were found to be 0.3–3.0 ng/mL in human blood and 0.06–0.6 ng/mL in urine. The recoveries of spiked target compounds at different concentrations in human blood and urine were 91.8–111.9% and 86.9–105.3%, respectively. Inter- and intra-day precision values were both less than 12.5%, and the matrix effects of human blood and urine samples for ARs were 75.3–108.6% and 102.7–130.0%, respectively. This method had successfully applied to the emergency detection of ARs in biological samples of poisoned patients.

3

Measurements of trace elements in human blood and urine using atomic emission spectrometry

Sakovich V. V., Boikov V. N., Lazareva A. M., Tsvirko M. P.

Chemistry, Environment, Biotechnology

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2019

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Vol. 22

20--25

EN

Arc-discharge atomic-emission spectrometry was used for determining trace amounts of metals in human blood and urine. Radiation spectra were recorded on an atomic-emission multichannel spectrometer AEMS. An optical multichannel analyzer (OMA) based on a photodiode array was used as the detector. The spectral resolution was characterized by the range 0.011 nm/diode and a spectral-line half-width no more than 0.033-0.044 nm. The samples were prepared for the measurements by the method of dry mineralization without acids. The obtained ash was mixed with a graphite powder in 3:7 mass ratio. For urine samples, the second variant of buffering a mixture of a graphite powder with potassium chloride (9.2 % of K) was also conducted. For determining the concentration of Pb, Cd, Cu and Zn in blood and the concentration of Co, Mn, Ni and Cu in urine three types of the calibrating mixtures containing, respectively, equal amounts of graphite powder and having predetermined concentrations of matrix elements (K, Na, Mg, Ca, Fe) were prepared. Lyphochek Urine Metals Control, Level 1 and Seronorm Trace Elements Urine was used as a reference material in determining trace amounts of elements in urine. Limits of detection were 0.13; 0.7 and 5.5 μg l-1 for Cd, Zn and Pb in blood and 1.2; 1.4; 1.5 and 1.9 μg l-1 for Ni, Mn, Co and Cu in urine respectively. The results obtained and the simplicity of preparation of samples for analysis, allow the conclusion that arc-discharge atomic-emission spectrometry can be used for determination of trace elements in human biological samples, forensic and clinical toxicology, screening investigations in ecologically adverse regions and workers in unhealthy industries.

4

Effect of activated carbon on methomyl poisoning by urine metabolomics base on gas chromatography–mass spectrometry

Li L., Hu L., Chen B., Dong Y., Lin Z., Wang Z., Wen C., Wang X., Wang S.

Acta Chromatographica

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2018

|

Vol. 30, no. 1

21--25

EN

In this study, we developed a urine metabolomic method by gas chromatography–mass spectrometry (GC–MS) combination with biomedical results to evaluate the effect of activated carbon on methomyl poisoning rats. The rats were divided into four groups, methomyl group, two activated carbon treatment group, and control group. According to the biochemical results, it indicated that activated carbon treated rats could cause liver and kidney function changes. According to the urine metabolomics results, activated carbon treatment group (10 min) and activated carbon treatment group (30 min) could be distinguished from methomyl group, and activated carbon treatment group (10 min) could be separated from activated carbon treatment group (30 min) rats, which indicated that the treatment of rats by activated carbon in different time had a different effect. The results indicate that metabolomic method by GC–MS may be useful to elucidate activated carbon treated on methomyl poisoning rats.

5

Opracowanie procedury oznaczania trzech związków z grupy farmaceutyków w próbkach moczu ludzkiego z wykorzystaniem procedury opartej na zastosowaniu techniki HPLC

Gnida A., Marciocha D., Turek-Szytow J.

Inżynieria i Ochrona Środowiska

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2017

|

T. 20, nr 4

429--445

EN

The aim of the study was to examine the possibility of determination and optimization of methodology for analysis of three selected drugs: trimethoprim, sulfamethoxazole and diclofenac in urine using high-performance liquid chromatography, without extraction of the pharmaceuticals to the solid phase. The chromatographic separation conditions were determined using a gradient elution system and mobile phase, which was a mixture of acetonitrile and a phosphate buffer, allowing detection of trimethoprim, sulfamethoxazole and diclofenac from 260, 210 and 310 μg/L respectively, and simultaneous determination of these analytes in the presence of urine components.

PL

Celem pracy było sprawdzenie możliwości i opracowanie metodyki oznaczania trzech wybranych leków: trimetoprimu, sulfametoksazolu i diklofenaku w moczu z wykorzystaniem wysokosprawnej chromatografii cieczowej (ang. high performance liquid chromatography, HPLC) bez uprzedniej ekstrakcji analitów do fazy stałej. Określono warunki rozdzielania chromatograficznego z zastosowaniem elucji gradientowej fazy ruchomej, którą była mieszanina acetonitrylu i buforu fosforanowego, co pozwoliło na detekcję trimetoprimu, sulfametoksazolu i diklofenaku odpowiednio na poziomie od 260, 210 i 310 μg/l i równoczesne oznaczenie tych analitów w obecności składników moczu.

6

Oznaczanie neopteryny w próbkach moczu wybranymi technikami analitycznymi

Waligóra A., Waligóra S., Damasiewicz-Bodzek A., Tyrpień-Golder K.

Analityka : nauka i praktyka

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2017

|

nr 2

54--60

PL

Opracowanie zwalidowanej procedury ilościowego oznaczania neopteryny w moczu stanowić może dobrą alternatywę dla testów immunoenzymatycznych.

7

Fast confirmation for marijuana metabolite: THC-COOH, ultra-fast LC—MS/MS run time, and application to routine samples

Zazoğlu S., Anilanmert B., Aydin M., Cengiz S.

Acta Chromatographica

|

2017

|

Vol. 29, no. 2

253--265

EN

A fast, reliable, inexpensive, and practical method with a low determination limit and high recovery has been developed for the determination of the marijuana metabolite in routine analysis. THC-COOH in urine was validated using liquid chromatography—tandem mass spectrometry (LC—MS/MS). Before an easy single-step extraction with Toxi-Tubes, basic hydrolysis was performed at 60 °C for 30 min. LC—MS/MS analysis takes 2.5 min for each sample, and the retention time of the analyte is 1.75 min. Specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, repeatability, and intermediate precision (inter-day) system suitability parameters were determined in the validation study. The recovery of the extraction method was 88.67 (±5.91). LOD and LOQ values were 1.41 and 5.00 ng mL−1, respectively. The method showed linear response between the values 5.00 and 500.00 ng mL−1. The repeatability was 9.64% (relative standard deviation, RSD%), and the intermediate precisions (RSDR%) were 10.73%, 13.74%, and 8.11% at 10.00, 100.00, and 200.00 ng mL−1 concentration levels, respectively. No statistically significant difference was found in ANOVA analysis, between three consecutive days in intermediate precision study, for 90% confidence level. HorRat values were between 0.34 and 0.61. The method was applied to CEDIA positive samples, obtained from the Trabzon Group Presidency of Turkish Council of Forensic Medicine, successfully.

8

Determination of nilotinib in spiked plasma, urine, and capsules by high-performance liquid chromatography with fluorimetric detection

Yilmaz E. M., Aydoğmuş Z., Aboul-Enein H. Y.

Acta Chromatographica

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2016

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Vol. 28, no. 3

313--331

EN

A precise and sensitive reversed phase high-performance thin-layer chromatography (RP-HPLC) method was developed for the determination of nilotinib (NTB) in spiked plasma, urine, and pharmaceutical capsule formulation. The method was based on derivatization NTB with 4-chloro-7-nitrobenzofurazan (NBD-Cl) in the borax buffer (pH 9). The method employs an isocratic elution using acetonitrile and 10 mM orthophosphoric acid (40:60 v/v) as a mobile phase and an C18 column (4.6 mm × 250 mm, 5 μm, Waters Symmetry), with a fluorescence detector (λex: 447 nm, λem: 530 nm). The method validation was performed with respect to linearity, recovery, accuracy, precision, and stability. The linear ranges were 100–600 ng mL−1 in standard solution, plasma, and urine. Correlation coefficients (r2) were higher than 0.9997 for all of the analytes, indicating good linear relationship. The percentage recovery was 87.89% for plasma, 95.35% for urine, and 96.07% for capsules.

9

Validation of the method for determination of plutonium isotopes in urine samples and its application in a nuclear facility at Otwock

Rzemek K., Czerwiński A., Dymecka M., Ośko J., Pliszczyński T., Haratym Z.

Nukleonika

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2015

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Vol. 60, No. 1

181--186

EN

The studies aimed at determining low activities of alpha radioactive elements are widely recognized as essential for the human health, because of their high radiotoxicity in case of internal contamination. Some groups of workers of nuclear facility at Otwock are potentially exposed to contamination with plutonium isotopes. For this reason, the method for determination of plutonium isotopes has been introduced and validated in Radiation Protection Measurements Laboratory (LPD) of the National Centre for Nuclear Research (NCBJ). In this method the plutonium is isolated from a sample by coprecipitation with phosphates and separated on a AG 1-X2 Resin. After electrodeposition, the sample is measured by alpha spectrometry. Validation was performed in order to assess parameters such as: selectivity, accuracy (trueness and precision) and linearity of the method. The results of plutonium determination in urine samples of persons potentially exposed to internal contamination are presented in this work.

10

Separacja uryny – dlaczego? jak? i co dalej?

Gnida A.

Gaz, Woda i Technika Sanitarna

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2015

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Nr 10

363--367

EN

Having in mind the sustainable development, the last decade is rich in new. The source-separation of urine and independent treatment of yellow wastewater represents new technical and technological solutions to improve the removal of nitrogen and phosphorus from wastewater, although stabilization of faeces for field fertilisation is known from ages. The article focuses on aims and some advantages and disadvantages of the urine source separation idea but at the most on the ways and opportunities of management of the collected human urine.

PL

Separacja moczu u źródła powstania i niezależne zagospodarowanie ścieków żółtych jest przykładem nowego nurtu mającego na celu poprawę usuwania azotu i fosforu ze ścieków i/lub niedopuszczenie do niekontrolowanego dostania się tych związków do środowiska, choć stabilizacja odchodów i ich wykorzystanie do nawożenia pól są znane od wieków. Artykuł stanowi przegląd doniesień ostatnich lat dotyczących celowości separacji uryny u źródła, wad i zalet tego pomysłu, a przede wszystkim sposobów i możliwości zagospodarowania zebranego moczu ludzkiego.

11

Badanie ogólne moczu – cz. I

Tisończyk J., Drożdż R.

Laboratorium - Przegląd Ogólnopolski

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2013

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nr 9-10

53--54

PL

Badanie ogólne moczu jest najstarszym testem laboratoryjnym wykonywanym wcześniej niż jakiekolwiek analizy krwi. Dzięki postępowi technologii uległo zmianie, ewoluując od subiektywnych ocen stanu pojedynczego pacjenta opartych na przesądach po nowoczesne, oparte na osiągnięciach chemii i elektroniki, wyniki ilościowe. Rozwój technologii pozwala na obiektywną analizę wielu parametrów równocześnie, kontrolę i standaryzację wyników i optymalizację kosztów tego popularnego badania.

EN

General urine test is an older laboratory analysis performed before any laboratory blood test. As a consequence of technology progress it subjected evolution from subjective based on superstitions analysis of the single patient to quantitative results based on achievements of modern chemistry and electronics. Progress in technology facilitates objective analysis of multiple results, quality control standardization and cost effectiveness of that popular laboratory test.

12

Badanie moczu - od starożytności do teraźniejszości

Szychowska K., Okrągła E., Gałęzowska G., Wolska L.

Analityka : nauka i praktyka

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2013

|

nr 1

73--76

PL

Mocz stanowi przedmiot zainteresowania od samych początków medycyny, jest cennym źródłem informacji o stanie zdrowia człowieka. Jego potencjał zauważono już w czasach starożytnych i przez wieki rozwijano metody służące poznaniu jego składu i przypisaniu ich do stanu zdrowia człowieka. W dobie poszukiwania nowych bezinwazyjnych metod oceny stanu zdrowia mocz przeżywa swój renesans, stanowiąc doskonały materiał do badania.

13

Badanie ogólne moczu ze szczególnym uwzględnieniem jego roli w okresie ciąży

Rodziewicz-Lurzyńska A., Bobilewicz D.

Laboratorium - Przegląd Ogólnopolski

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2012

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nr 9-10

44--46

PL

Badanie ogólne moczu jest jednym z podstawowych badań laboratoryjnych służących do ogólnej oceny stanu zdrowia. Pozwala uzyskać zarówno informacje dotyczące pierwotnych chorób układu moczowego (zakażenia, kamica, choroby nerek o różnej etiologii), jak i zaburzeń ogólnoustrojowych (cukrzyca, nadciśnienie, miażdżyca). Szczególną rolę ma ono w okresie ciąży, kiedy może dotarczyć istotnych informacji diagnostycznych (białkomocz, glukozuria, leukocyturia) odnośnie potencjalnych zagrożeń dla matki i płodu (poród przedwczesny, stan przedrzucawkowy).

EN

Urinalysis is one of the basic laboratory tests to assess general health. It as well provides information regarding primary renal and urinary tract diseases (infection, lithiasis, renal disease of different origin) as concerning general disorders (diabetes, hypertension, atherosclerosis). It plays important role in pregnancy as it can give essential diagnostic data (proteinuria, glucosuria, leukocyturia) about potential threat for mother and fetus (preterm labor, preeclampsia).

14

Determination of nalidixic acid using dispersive liquid-liquid microextraction followed by HPLC-UV

Daneshfar A, Lotfi H. J, Khezeli T

Acta Chromatographica

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2011

|

Vol. 23, no. 4

567--577

EN

A fast, simple, and sensitive sample preparation procedure based on dispersive liquid-liquid microextraction (DLLME) followed by high-performance liquid chromatography and ultraviolet (HPLC-UV) detection was developed for the determination of nalidixic acid in a human urine sample. A mixture of extraction solvent (35 μL carbon tetrachloride) and disperser solvent (1.0 mL acetonitrile) were rapidly injected into an aqueous sample (5.0 mL) for the formation of cloudy solution; the analyte in the sample was extracted into the fine droplets of carbon tetrachloride. After extraction, phase separation was performed by centrifugation and the enriched analyte in the sedimented phase was determined by HPLC-UV. The influence of several important parameters on extraction efficiency of nalidixic acid was evaluated. Under optimized experimental conditions, the calibration graph was linear in the concentration range of 1–800 μg L-1 with the coefficient of determination being 0.9994. The limits of detection and quantification were 0.2 and 0.7 μg L-1, respectively. The relative standard deviations (RSDs) and accuracies were in the range of 1.1–8.7% and 92.7–104.9%, respectively. This procedure was successfully applied to the determination of nalidixic acid in spiked urine samples with satisfactory results. The relative recoveries of urine samples ranged from 103.1% to 105.1%, with RSDs varying from 0.8% to 2.4%.

15

Chemical communication in mammal population : urinary olfactory chemosignals in lactating female root voles (Microtus oeconomus Pallas)

Yu H., Zhao X., Yue P., Sun P.

Polish Journal of Ecology

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2010

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Vol. 58, nr 1

153-165

EN

Urine is a major source of mammalian chemosignals. Among rodents, the sexual attractiveness and chemical constituents of urine vary with different reproductive stages. We confirmed the differing sexual attractiveness to males of the urine of lactating and non-lactating female root voles (Microtus oeconomus) and analyzed individual coding forms and lactation-specific putative pheromones, using gas chromatography-mass spectrometry (GC-MS). First, we documented the behavioral preference of male voles to urine odors of lactating and non-lactating females in a choice maze. The results showed that male voles engaged in more sniffing behavior and spent more time self-grooming in response to urinary odors of lactating females than to urinary odors of non-lactating females. We then used GC-MS to analyze the urine.s individual coding forms and potential chemosignals. We identified 34 volatile compounds, corresponding to 34 GC peaks, in the urine of female voles. The components identified in the urine samples included benzo- forms, alkanes, alkenes, acids, esters, pyrans, alcohols, and other volatile compounds. 12 basic volatiles were detected in all urine samples while others were specific to individuals. (E)5-octadecene and (N) hexadecanoic acid were specific to the lactating stage. A quantitative comparison of the relative abundances of the basic GC peaks showed no difference between the lactating and non-lactating stages, suggesting that individual identity is coded in digital form. We suggest that the urine of lactating females possesses stronger sexual attraction cues because of the presence of (E)5-octadecene and (N)hexadecanoic acid, which are putative lactating pheromones. However, the specific function of the pheromones should be assessed further by bioassay.

16

Profilowanie metabolitów prób moczu noworodków

Schneider B., Zurek G., Baessmann C., Schaefer H., Godejohann M., Keller S., Spraul M., Fusch G., Nauck M., Fusch Ch., Rucińska M., Karpiński A.

Laboratorium - Przegląd Ogólnopolski

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2009

|

nr 7-8

40--41

PL

Wrodzonym wadom metabolizmu poświęca się sporo uwagi nie tylko ze względu na ich znaczenie, ale również dlatego, że reprezentują one uniwersalny system pozwalający zademonstrować korzyści profilowania metabolitów. W niniejszym opracowaniu do analizy próbek moczu noworodków użyto systemu profilowania metabolitów opartego na technikach LC-MS oraz MR. Identyfikacji związków chemicznych w próbkach moczu noworodków dokonano bez żadnej wiedzy a priori o leczeniu, w podwójnie ślepej próbie.

EN

In born errors of metabolism receive much attention due to their clinical relevance, but they also represent a versatile system to demonstrate the benefits of metabolic profiling. A metabolic profiling system based on LC-MS and MR has been developed and applied to child urine samples. The identification of chemical compounds from the baby urine samples was achieved without any prior knowledge of treatment in a double blind experiment.

17

In-situ plated lead film electrode for determination of glipizide in pharmaceutical formulation and human urine

Tyszczuk K., Korolczuk M.

Chemia Analityczna

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2009

|

Vol. 54, No. 1

31-41

EN

In this paper, electrochemical behavior of glipizide at an in-situ plated lead film electrode has been studied. A simple and precise square wave adsorptive stripping voltammetric procedure for quantification of glipizide with detection limit of 2.5 x 10-9 mol L-1 has been described. Relative standard deviation for determination of 5 x 10-9mol L-1 glipizide was 3.5%. The measurements were carried out in non-deoxygentaed solutions. The proposed procedure has been successfully applied to quantification of glipizide in its pharmaceutical formulations and human urine samples.

PL

W pracy zbadano elektrochemiczne zachowanie się glipizidu na tworzonej in-situ błonkowej elektrodzie ołowiowej. Opisano prostą i precyzyjną procedurę oznaczania glipizidu z wykorzystaniem adsorpcyjnej woltamperometrii stripingowej i techniki fali prostokątnej, o granicy wykrywalności równej 2,5 x 10-10mol L-1. Względne odchylenie standardowe oznaczania glipizidu o stężeniu 5 x 10-9 mol L-1wynosiło 3,5%. Pomiary przeprowadzono w roztworach nieodtlenionych. Zaprezentowana procedura została zastosowana do oznaczania glipizidu ,, w preparatach farmaceutycznych i próbkach ludzkiego moczu.

18

Easy and accurate determination of urea in milk, blood plasma, urine and selected diets of mammals by high-performance liquid chromatography with photodiode array detection preceded by pre-column derivatization

Czauderna M., Kowalczyk J.

Chemia Analityczna

|

2009

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Vol. 54, No. 5

919-937

EN

An HPLC method with photodiode array detection for simple and rapid determination of urea in physiological fluids of domestic animals has been described. A physiological fluid (blood plasma, urine, or milk) was treated with 20% trichloroacetic acid and then the mixture was centrifuged. 200 &muL of the supernatant were derivatized using 50 uL of p-dime-thylaminobenzaldehyde (DMAB) dissolved in HC1 (1.3 g DMAB in 10 mL of 20% HC1). ' The derivatized samples were ready for HPLC analysis. Derivatized urea in standards and biological samples was analyzed using a Nova-Pak C18 column (4 &mum, 300 * 3.9 mm, Waters, USA). A ternary gradient elution program and UV detection at 255 and 414 nm were applied for urea analyses. Clear separation of urea from endogenous species present in biological materials was achieved in less than 20 min. Elution of derivatized urea was confirmed by an unsymmetrical chromatographic peak at 9.67 š0.11 min, which was a combination of two poorly resolved urea peaks eluted at 8.54 š 0.07 and 9.84 š 0.08 min. ; -' Average recoveries of urea standards added to the assayed biological materials were satisfactory, especially when detection at 414 nm (101.2%) was applied. Precision of the method with detection at 255 nm was inferior (CV 2.65%) to that performed at 414 nm (CV 1.98%). The proposed method with UV monitoring at 255 and 414 nm offers low detection limits (5.62 and 43 ng, respectively) and quantification limits (18.7 and 142 ng, respectively). It provides satisfactory accuracy, precision, and sensitivity of determination of urea. Liquid chromatography with UV monitoring at 255 nm revealed that the presence of endogenous substances in the assayed biological materials affect accurate and precise integration of the

PL

Opisano metodę HPLC pozwalającą na proste i szybkie oznaczanie mocznika w płynach fizjologicznych pozyskiwanych od zwierząt gospodarskich. W metodzie tej do detekcji wykorzystano detektor z matrycą diodową. Do płynów fizjologicznych (osocze krwi, mocz i mleko) dodawano 20%kwas trichlorooctowy; następnie uzyskanąmieszaninę wirowano. Do 200 μL supernatantu dodawano 50 &muL p-dimetyloaminobenzaldehydu (DMAB) w HC1 (l .3 g DMAB w l0 mL 20%HC1). Pochodna mocznika w badanych próbkach była gotowa do analizy. Pochodną mocznika analizowano przy użyciu kolumny Nova Pak Cl18 (4 μm, 300 x 3.9 mm, Waters). Zastosowano elucję gradientową! wykrywanie przy długości fali 255 i 414 nm. Zadowalające rozdzielenie mocznika od endogennych składników próbek uzyskano w czasie krótszym niż 20 min. Pochodna mocznika, jako niesymetryczny pik, pojawiła się w 9,67 š0,11 min; pik ten był kombinacją dwóch pików pojawiających się w 8,54 š 0,07 oraz 9,84 š 0,08 min. Średni odzysk wzorców mocznika dodanych do badanych próbek był zadowalający (101,2%), szczególnie przy detekcji UV przy długości fali 414 nm. Precyzja oznaczania mocznika przy długości fali 255 nm jest gorsza (CV = 2,65%) od precyzji oznaczania przy długości fali 414 nm (CV = 1,98%). Przy długości fali 255 i 414 nm otrzymano wykrywalność i oznaczalność wynoszące odpowiednio 5.62 oraz 43 ng oraz 18,7 i 142 ng. Opracowana metoda pozwala na oznaczenie mocznika z zadowalającą dokładnością, precyzjąoraz czułością. Chromatografia cieczowa z detekcjąprzy długości fali 255 nm ujawnia obecność endogennych substancji, które utrudniaj ą dokładne i precyzyjne oznaczanie mocznika w badanych próbkach biologicznych. Opracowana metoda z detekcją przy długości fali 414 nm analitycznąpozwalającąna proste i szybkie oznaczanie mocznika w płynach fizjologicznych oraz wybranych paszach.

19

Analysis of major urinary aminothiols by high-performance liquid chromatography with ultraviolet detection

Kuśmierek K, Bald E.

Acta Chromatographica

|

2009

|

Vol. 21, no. 3

411--420

EN

High-performance liquid chromatography has been used for measurement of the concentrations of total cysteine and cysteinylglycine in human urine. The method involved conversion of disulfides to their reduced counterparts by use of tris(2-carboxyethyl)phosphine hydrochloride, derivatization with 1-benzyl-2-chloropyridinium bromide, and ion-pairing reversed-phase high-performance liquid chromatographic separation with ultraviolet detection at 315 nm. The linearity of the method was validated in the ranges 50–300 and 5–50 µmol L -1 urine for cysteine and cysteinylglycine, respectively; regression coefficients were better than 0.999. The detection and quantitation limits were 0.2 and 0.5 µmol L -1, respectively, for both analytes. Intra-assay and inter-assay imprecision were below 6.0%, and accuracy was 98.95–100.80%. The method was applied to urine samples donated by apparently healthy volunteers.

20

Skład moczu jako źródło informacji o narażeniu zawodowym na związki organiczne

Rutkiewicz I., Namieśnik J.

Ecological Chemistry and Engineering. S

|

2008

|

Vol. 15, nr 4

561-585

PL

Przedstawiono przegląd prac dotyczących wykorzystania próbek moczu ludzkiego do badań analitycmych prowadzonych w celu uzyskania informacji o ekspozycji zawodowej na związki organiczne. Toksyczne działanie większości z tych związków stwarza nadal duże zagrożenie wystąpienia chorób zawodowych. Stąd też bardzo ważne jest wykorzystanie monitoringu biologicznego do oceny ryzyka zawodowego. Przedstawiono również najczęściej stosowane techniki izolacji i wzbogacania związków organicznych i ich metabolitów z próbek moczu, a także techniki omaczania analitów w otrzymanych ekstraktach.

EN

Information about the possibility of employing human urine samples as a material for analytical research directed toward obtaining information on occupational exposure to organic compounds was presented. Most compounds have toxic action, what generates high risk of occupational disease. Therefore it is very important to use the biological monitoring to assess occupational exposure. Techniques of isolation and/or enrichment of organic compounds and their metabolites from the urine samples, techniques used to determine organic compounds in the extracts are presented and discussed.