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1

Simultaneous determination of dantrolene with ibuprofen and diclofenac in plasma by HPLC-DAD: Application to comparative pharmacokinetic study

Abdel Moneim Mona M.

Acta Chromatographica

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2024

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Vol. 36, no. 1

23--30

EN

Muscle relaxants and pain killers with their different types are widely used as combination approach for treatment of pain associated with several muscle spasm conditions. A sensitive and simple HPLC-UV detection method was developed in this work for simultaneous assay of Dantrolene (DNT) and co-administrated: Ibuprofen (IBU) and Diclofenac (DIC). After simple protein precipitation, separation was achieved using C₁₈ column (150 × 4.6 mm) with a mobile phase of acidified water with orthophosphoric acid (pH = 3.5) and acetonitrile using gradient elution with a flow rate of 1 mL/min. The DAD was adjusted at 380, 219, 280 and 240 nm to measure DNT, IBU, DIC, and dexamethasone (internal standard), respectively. Linearity was demonstrated over the range from 0.1 to 3 μg/mL, 1 to 40 μg/mL, and 0.1 to 2 μg/mL for DNT, IBU, and DIC, respectively. The validated method was applied successfully to compare the effect of co-administration of IBU or DIC on the pharmacokinetic profile of DNT.

2

Using Design Space and Response Surface Methodology for developing a liquid chromatography method for simultaneous determination of five statins in pharmaceutical form

Belmir H., Abourriche A., Bennamara A., Saffaj T., Ihssane Bouchaib

Acta Chromatographica

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2021

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Vol. 33, no. 4

345--353

EN

This study describes the development of a method allowing the simultaneous separation and quantification of five statins by High performance liquid chromatography/Diode Array Detector (HPLC/ DAD). Optimization was accomplished using chemometric tools such as the Design Space (DS) and Response Surface Methodology (RSM). Central Composite Design (CCD) and DS were applied for the optimization of the chromatographic procedure as well as the robustness of the chromatographic method by taking the ratio of the percentage of acetonitrile (%ACN) Buffer solution, the pH and the mobile phase flow rate as critical parameters. Satisfactory results were obtained after the optimization phase with a percentage of mobile phase equal to 46.19%, a pH of 4.16 and the flow rate is 1.4 mL min1 by setting the resolution limits above 6, and the target retention time of 20 min. Using the DS and CCD approach, we have developed a robust and reliable procedure for the simultaneous and accurate separation and quantification of the five statins.

3

Extraction process and method validation for bioactive compounds from Citrus reticulata cv. Chachiensis : application of response surface methodology and HPLC–DAD

Mei Zhenying, Zhang Rongfei, Zhao Zhimin, Zheng Guodong, Xu Xinjun, Yang Depo

Acta Chromatographica

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2021

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Vol. 33, no. 3

270--280

EN

Citrus reticulata cv. Chachiensis, a traditional Chinese herb, has extensive medicinal and edible effects. 3′,4′,5,6,7,8-Hexamethoxyflavone (HM) and 5,6,7,8,4′-pentamethoxyflavone (PM) are main bioactive compounds in Chachiensis, which have been reported to possess various biological properties. In this study, supercritical CO2 extraction (SCE) and high-speed countercurrent chromatography (HSCCC) were utilized to prepare HM and PM from Chachiensis. The contents of target compounds were determined by a high-performance liquid chromatography method with diode-array detection (HPLC-DAD), which was validated using the following parameters: linearity, sensitivity, repeatability, stability, precision and accuracy. The SCE conditions were optimized using response surface methodology with central composite design. Obtained optimum conditions were temperature of 37.9 °C, pressure of 26.3 MPa, and modifier volume of 81.0 mL. Under above conditions, the recoveries of target compounds were 92.52 ± 0.83 and 96.36 ± 0.43%, respectively. The most appropriate solvent system for HSCCC was selected as n-hexane/ethyl acetate/methanol/water (1:0.8:1:1.2, v/v). The HSCCC fractions were detected by HPLC-DAD, liquid chromatography-mass spectrometry (LC-MS) and nuclear magnetic resonance spectroscopy (1H NMR and 13C NMR). The results indicated that this method was successfully applied to obtain HM and PM with high purities and high recoveries from Chachiensis.

4

A reliable HPLC-DAD method for simultaneous determination of related substances in TBI-166 active pharmaceutical ingredient

Zhang Tingting, Yin Wanting, Jin Bo, Li Tong, Ma Chen

Acta Chromatographica

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2020

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Vol. 32, no. 2

80--85

EN

A sensitive, stability-indicating reversed-phase high-performance liquid chromatography with diode array detection (HPLC–DAD) method has been developed for the determination of TBI-166 and its 10 kinds of related impurities. Chromatographic separation was achieved on a Kromasil ODS column (250 mm × 4.6 mm, 5 μm), with a gradient elution of the mobile phase system consisting of acetonitrile and 1% ammonium formate solution (with 0.2% formic acid). The flow rate was 1.0 mL/min, and the detection wavelength was set at 251 nm. The method was validated according to the International Conference on Harmonization (ICH) guidelines with respect to selectivity, linearity, limits, accuracy, precision, and robustness. The calibration curves were linear from LOQ to 150% of the specification limit of impurity with correlation coefficients not less than 0.999. The limits of quantitation were between 0.123 and 0.257 μg/mL. Accuracy for the related substances was estimated by the recovery ranged from 94.6% to 111.2%. The method was proved to be reliable for the determination of related substances in TBI-166 bulk drug, which is essential and important in the quality control.

5

Development and validation of a rapid HPLC method for multiresidue determination of erythromycin, clarithromycin, and azithromycin in aquaculture fish muscles

Habibi B., Ghorbel-Abid I., Lahsini R., Ben Hassen D. Chehimi, Trabelsi-Ayadi M.

Acta Chromatographica

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2019

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Vol. 31, no. 2

109--112

EN

An accurate, sensitive, and reproducible high-performance liquid chromatographic method with diode array detection has been developed for simultaneous determination of erythromycin, clarithromycin, and azithromycin residues in fish muscles. Analysis was carried out using a Shodex Asahipak high-performance liquid chromatography (HPLC) column, monitoring was at 210 nm and a mobile phase consisting of a mixture of acetonitrile and phosphate buffer (pH 11 ± 0.05) in the ratio of 60:40 (v/v). Solid-phase extraction method was used in samples extraction and purification. Recoveries were in the range 72.0–92.2% with relative standard deviation (RSD) from 2.3% to 8.3%. This method was validated for fish muscles in aquaculture following the commission decision 2002/657/EC criteria. It is demonstrated that the new method is robust for detection and quantification of the three macrolides residues. Decision limit (CCα) was from 214 to 228 μg/kg and capacity of detection (CCβ) was from 228 to 256 μg/kg.

6

Application of mobile phases containing ionic liquid for the analysis of selected psychotropic drugs by HPLC–DAD and HPLC–MS

Petruczynik A., Wróblewski K., Waksmundzka-Hajnos M.

Acta Chromatographica

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2019

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Vol. 31, no. 4

255--261

EN

In reversed-phase liquid chromatography, in case of the absence of additives, cationic basic compounds give rise to asymmetrical and broad peaks as a result of interactions of analyte cations with residual free silanols on silica-based stationary phases. Ionic liquids, added to the mobile phase, have been suggested as alternatives to amines to block the activity of free silanols. The different parameters affecting the retention behavior, symmetry of peak, system efficiency, and separation selectivity of selected psychotropic drugs, especially the effect of concentration of ionic liquid, kind and concentration of organic modifiers of mobile phases, and kind of stationary phases were investigated. The most selective and efficient systems are used for separations of psychotropic drug standards' mixture and for determination of selected psychotropic drugs in human serum.

7

Bezwodnik maleinowy : oznaczanie w powietrzu na stanowiskach pracy

Woźnica A.

Podstawy i Metody Oceny Środowiska Pracy

|

2017

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Nr 1 (91)

115--125

PL

Bezwodnik maleinowy jest krystalicznym ciałem stałym, ważnym półproduktem w przemyśle chemicznym. Bezwodnik maleinowy jest substancją: szkodliwą, drażniącą i uczulającą. Celem pracy było opracowanie nowej metody oznaczania stężeń bezwodnika maleinowego w powietrzu na stanowiskach pracy w zakresie od 1/10 do 2 wartości NDS, zgodnie z wymaganiami zawartymi w normie PN-EN 482. Badania wykonano, stosując chromatograf cieczowy (HPLC) serii 1200 firmy Agilent Technologies z detektorem diodowym (DAD). Oznaczenia prowadzono w układzie faz odwróconych (faza ruchoma: acetonitryl: roztwór kwasu fosforowe-go(V)) z zastosowaniem kolumny Ultra C18 (250 x 4,6 mm o dp = 5 μm). Metoda polega na: za-trzymaniu obecnego w powietrzu bezwodnika maleinowego na filtrze z włókna szklanego z naniesioną 3,4-dimetoksybenzyloaminą i ftalanem dioktylu, ekstrakcji utworzonej pochodnej wodnym roztworem amoniaku i analizie chromatograficznej otrzymanego roztworu. Na podstawie wyników badań ustalono warunki oznaczania bezwodnika maleinowego w powietrzu na stanowiskach pracy w zakresie stężeń 0,05 ÷ 1 mg/m³. Walidację metody przeprowadzono zgodnie z wymaganiami zawartymi w normie europejskiej PN-EN 482. Uzyskano następujące dane walidacyjne: granica wykrywalności, LOD 8,18 ng/ml granica oznaczalności, LOQ 24,5 ng/ml całkowita precyzja badania 5,53% względna niepewność całkowita 12,02%. Opracowana metoda umożliwia selektywne oznaczanie bezwodnika maleinowego w powietrzu na stanowiskach pracy w zakresie stężeń 0,05 ÷1 mg/m3, czyli od 1/10 do 2 wartości NDS w obecności substancji współwystępujących w badanym powietrzu. Metoda charakteryzuje się dobrą precyzją i dokładnością, spełnia wymagania zawarte w normie europejskiej PN-EN 482 dla procedur oznaczania czynników chemicznych. Opracowaną metodę oznaczania bezwodnika maleinowego zapisano w postaci procedury analitycznej, którą zamieszczono w załączniku.

EN

Maleic anhydride is a crystalline solid. Maleic anhydride is an important intermediate in the chemical industry. It is harmful, irritating and sensitizing. The aim of this study was to develop a new method for determining concentrations of maleic anhydride in workplace air in the range from 1/10 to 2 MAC values, in accordance with the requirements of Standard No. EN 482. The study was performed using a liquid chromatograph ( Agilent Technologies series 1200) with a diode array detector (DAD). The determination was performed in the reverse-phase system (mobile phase: acetonitrile: solution of phosphoric acid) using an Ultra C18 column (250 × 4.6 mm with dp = 5 μm) with precolumn (10 × 4 mm). The method was based on passing air through a glass fiber filter coated with 3,4-di-methoxybenzylamine and di-noctyl phthalate. Samples were extracted with aqueous ammonium hydroxide and analyzed with HPLC. The method was validated according to Standard No. EN 482. The measuring range was 0.05  1 mg/m3 , the limit of detection (LOD) was 8.18 ng/ml, the limit of quantification (LOQ) was 24.5 ng/ml, the overall accuracy of the method was 5.53% and the relative total uncertainty of the method was 12.02%. The analytical method described in this paper enables selective determination of maleic anhydride in workplace air in the presence of other substances at concentrations from 0.05 mg/m³ (1/10 MAC value). The method is precise, accurate and it meets the criteria for measuring chemical agents listed in Standard No. EN 482. The developed method of determining maleic anhydride has been recorded as an analytical procedure (see appendix).

8

Simultaneous determination of eleven alkaloids in Corydalis decumbens by HPLC with diode-array detection

Gu G. H., Yang D. J., Wang S. Y., Zeng W., Wang W., Yuan J. S.

Acta Chromatographica

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2017

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Vol. 29, no. 1

121--134

EN

A high-performance liquid chromatography—diode-array detection method was developed and validated to determine simultaneously eleven major alkaloids in Corydalis decumbens (Thunb.) Pers. The alkaloids detected were corlumidine, protopine, coptisine, tetrahydrojatrorrhizine, palmatine, berberine, sanguinarine, papaverine hydrochloride, tetrahydropalmatine, bicuculline, and corydaline. Chromatographic separation was achieved using a C-18 column with a mobile phase composed of A (0.2% acetic acid solution, adjusted with triethylamine to pH 5.0) and B (acetonitrile), with stepwise gradient elution. Ultraviolet diode-array detection was used; chromatograms were examined at the wavelength of 280 nm. The regression equations showed a good linear relationship between the peak area of each marker and concentration (r = 0.9994–0.9999). The recovery values ranged between 93.66% and 100.54%. The method was fully validated with respect to detection and quantification limits, precision, reproducibility, and accuracy. The described high-performance liquid chromatography (HPLC) method was successfully used for the differentiation and quantification of the eleven major alkaloids in C. decumbens (Thunb.) Pers. and can be considered an effective procedure for the analyses of this important class of natural compounds.

9

Development and validation of an isocratic HPLC method for simultaneous determination of quaternary mixtures of antihypertensive drugs in pharmaceutical formulations

Anderson J. F. F., Gerlin M. C. G., Sversut R. A., Oliveira L. C. S., Singh A. K., Amaral M. S., Kassab N. M.

Acta Chromatographica

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2017

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Vol. 29, no. 1

95--110

EN

The objective of this study was to develop and validate an assay method for simultaneous determination of atenolol, furosemide, losartan, and spironolactone in pharmaceutical formulations. A reverse-phase high-performance liquid chromatography procedure was developed, using a Kinetex® C-18 column (100 mm × 4.6 mm, 2.6 μm). The mobile phase was composed of metanol-water (75:25 v/v, pH 3.0, adjusted with phosphoric acid), with a flow rate of 0.4 mL min-1. All drugs were separated in less than 5 min. The method was validated according to International Conference on Harmonization (ICH) and Association of Official Analytical Chemists (AOAC) guidelines. The method showed linearity in a concentration range of 0.75–12.0 μg Ml-1 for atenolol (r = 0.9995), 0.30–12.00 μg Ml-1 for furosemide (r = 0.9997), 0.45–12.00 μg Ml-1 for losartan (r = 0.9995), and 0.45–12.0 μg Ml-1 for spironolactone (r = 0.9999). The method also showed repeatability and precision. The three-day average intra-day precisions were 101.35 ± 0.74% for atenolol, 95.84 ± 1.44% for furosemide, 98.90 ± 1.16% for losartan, and 97.19 ± 0.18% for spironolactone. Similarly, the inter-day precisions were 101.34 ± 0.72% for atenolol, 95.84 ± 0.1.50% for furosemide, 98.90 ± 1.17% for losartan, and 97.19 ± 0.83% for spironolactone. The method accuracy was also tested and validated - in this case, the average recovery values were 100.18 ± 1.20% for atenolol, 99.83 ± 1.54% for furosemide, 100.07 ± 0.95% for losartan, and 99.94 ± 0.93% for spironolactone. Finally, the method was successfully applied in the simultaneous determination of atenolol, furosemide, losartan, and spironolactone in magisterial formulas, as well as in commercial pharmaceutical formulations.

10

Determination of vortioxetine in human serum and saliva samples by HPLC–DAD and HPLC–MS

Wróblewski K., Petruczynik A., Buszewski B., Szultka-Młyńska M., Karakuła-Juchnowicz H., Waksmundzka-Hajnos M.

Acta Chromatographica

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2017

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Vol. 29, no. 3

325--344

EN

Vortioxetine is a new drug against major depressive disorder with high affinity for a range of different serotonergic targets in the central nervous system. Therapeutic drug monitoring is an important tool for the clinical management of patients receiving a pharmacotherapy, particularly in psychiatry. For this reason, determination of drug concentration in biological fluids is important for a rational dosage of drugs. Rapid and reliable analytical assays are also required to detect and identify drugs of toxicological importance. For analysis of vortioxetine by high-performance liquid chromatography (HPLC), no procedures for its determination in saliva have been reported and there are only a few ones for its determination in serum. A sensitive and selective highperformance liquid chromatography with diode array detector (HPLC-DAD) or mass spectrometer (HPLC-MS) method was developed for the fast quantification of vortioxetine in human saliva and serum. The determination was performed on a Synergi Polar RP column in isocratic mode under the optimal mobile phase containing 70% methanol, 20% acetate buffer at pH 3.5, 10% double distilled water, and 0.025 M L−1 diethylamine.

11

Bezwodnik ftalowy : oznaczanie w powietrzu na stanowiskach pracy

Woźnica A.

Podstawy i Metody Oceny Środowiska Pracy

|

2016

|

Nr 1 (87)

33--45

PL

Bezwodnik ftalowy jest krystalicznym ciałem stałym. Związek jest ważnym półproduktem w przemyśle chemicznym. Bezwodnik ftalowy jest substancją: szkodliwą, drażniącą i uczulającą. Celem pracy było opracowanie nowej metody oznaczania stężeń bezwodnika ftalowego w powietrzu na stanowiskach pracy w zakresie od 1/10 do 2 wartości najwyższego dopuszczalnego stężenia (NDS), zgodnie z wymaganiami zawartymi w normie europejskiej PN-EN 482. Badania wykonano stosując chromatograf cieczowy (HPLC) serii 1200 firmy Agilent Technologies z detektorem diodowym (DAD). Oznaczenia prowadzono w układzie faz odwróconych – faza ruchoma: acetonitryl: roztwór kwasu fosforowego(V) z zastosowaniem kolumny Ultra C18(250 x 4,6 mm o dp = 5 μm). Metoda polega na: zatrzymaniu obecnego w powietrzu bezwodnika ftalowego na filtrze z włókna szklanego z naniesioną 3,4-dimetoksybenzyloaminą i ftalanem dioktylu, ekstrakcji utworzonej pochodnej wodnym roztworem amoniaku i analizie chromatograficznej otrzymanego roztworu. Na podstawie wyników przeprowadzonych badań ustalono warunki oznaczania bezwodnika ftalowego w powietrzu na stanowiskach pracy w zakresie stężeń 0,1 ÷ 2 mg/m³. Walidację metody przeprowadzono zgodnie z wymaganiami zawartymi w normie europejskiej PN-EN 482. Uzyskano następujące dane walidacyjne: − granica wykrywalności, LOD 9,91 mg/ml (0,000137 mg/m3 dla próbki powietrza 720 l) − granica oznaczalności, LOQ 29,74 mg/ml dla próbki powietrza 720 l) całkowita precyzja badania 5,31% − względna niepewność całkowita 11,63%. Metoda analityczna umożliwia selektywne oznaczanie bezwodnika ftalowego w powietrzu na stanowiskach pracy w zakresie stężeń od 0,1 mg/m3 (1/10 wartości NDS) w obecności substancji współwystępujących w badanym powietrzu. Metoda charakteryzuje się dobrą precyzją i dokładnością, spełnia wymagania zawarte w normie europejskiej PN-EN 482 dla procedur oznaczania czynników chemicznych. Opracowaną metodę oznaczania bezwodnika ftalowego zapisano w postaci procedury analitycznej, którą zamieszczono w załączniku.

EN

Phthalic anhydride is a crystalline solid. Phthalic anhydride is an important intermediate in the chemical industry. It is harmful, irritating and sensitizing.The aim of this study was to develop a new method for determining concentrations of phthalic anhydride in workplace air in the range from 1/10 to 2 MAC values, in accordance with the requirements of Standard No. EN 482.The study was performed using an liquid chromatograph (Agilent Technologies series 1200) with a diode array detector (DAD). The determination was performed in the reverse-phase system (mobile phase: acetonitrile: solution of phosphoric acid) using an Ultra C18 column (250 × 4.6 mm with dp= 5 μm) and with precolumn (10 × 4 mm).The method is based on passing air through a 3,4-dimethoxybenzylamine-coated glass fiber filter. Samples were extracted with acetonitrile/ammonia and analyzed with HPLC-DAD. The procedure was validated according to Standard No. EN 482. The measuring range was 0,1 ÷ 2 mg/m3, the limit of detection (LOD) was 9.91 ng/ml (0.000137 mg/m3a 720-L air sample), the limit of quantification (LOQ) was 29.74 mg/ml (0.000413 mg/m3a 720-L air sample), the overall accuracy of the method was 5.31% and the relative total uncertainty of the method was 11.63%.The analytical method described in this paper enables selective determination of phthalic an-hydride in workplace air in the presence of other compounds at concentrations from 0.1 mg/m³ (1/10 MAC value). The method is precise, accurate and it meets the criteria for procedures for measuring chemical agents listed in Standard No. EN 482. The developed method of determining phthalic anhydride has been recorded as an analytical procedure (see Appendix).

12

Akrylamid : oznaczanie w powietrzu na stanowiskach pracy

Jeżewska A.

Podstawy i Metody Oceny Środowiska Pracy

|

2016

|

Nr 1 (87)

15--17

PL

Akrylamid jest bezwonnym, białym i krystalicznym ciałem stałym, dobrze rozpuszczalnym w rozpuszczalnikach polarnych (woda, etanol). Jest to substancja syntetyczna stosowana w wielu dziedzinach przemysłu, głównie do produkcji poliakrylamidu. Międzynarodowa Agencja Badań nad Rakiem (IARC) zaklasyfikowała akrylamid do grupy związków prawdopodobnie rakotwórczych dla ludzi. Celem pracy było opracowanie metody oznaczania stężeń akrylamidu w powietrzu na stanowiskach pracy w zakresie 1/10 ÷ 2 wartości najwyższego dopuszczalnego steżenia (NDS), zgodnie z wymaganiami zawartymi w normie europejskiej PN-EN 482. Badania wykonano przy zastosowaniu chromatografu cieczowego (HPLC) serii 1200 firmy Agilent Technologies z detektorem diodowym (DAD), rejestrującym sygnał przy długości fali analitycznej, którą zamieszczono w załączniku.

EN

Acrylamide is an odourless, white crystalline solid, highly soluble in polar solvents (e.g., water, ethanol). Acrylamide is a synthetic compound widely used in several industries but particularly in the production of polyacrylamide. International Agency for Research on Cancer (IARC) classified acrylamide as a probably carcinogenic to humans.The aim of this study was to develop a method for determining concentrations of acrylamide in workplace air in the range from 1/10 to 2 MAC values, in accordance with the requirements of Standard No. EN 482.The study was performed using an liquid chromatograph (Agilent Technologies series 1200) with a diode array detector (DAD) with an analytical wavelength of 195 nm and 208 nm.

13

2-Metylo-4,6-dinitrofenol : oznaczanie w powietrzu na stanowiskach pracy

Jeżewska A.

Podstawy i Metody Oceny Środowiska Pracy

|

2016

|

Nr 1 (87)

109--122

PL

2-Metylo-4,6-dinitrofenol (DNOC) jest żółtym ciałem stałym. Substancja ta działa: owadobójczo, grzybobójczo i chwastobójczo. Obecnie 2-metylo-4,6-dinitrofenol jest stosowany głównie jako inhibitor polimeryzacji oraz produkt pośredni w przemyśle chemicznym. Jest substancją bardzo toksyczną dla ludzi. Celem pracy było opracowanie nowej metody oznaczania stężeń 2-metylo-4,6-dinitrofenolu w powietrzu na stanowiskach pracy w zakresie od 1/10 do 2 wartości NDS zgodnie z wymaganiami zawartymi w normie europejskiej PN-EN 482. Badania wykonano, stosując chromatograf cieczowy (HPLC) serii 1200 firmy Agilent Technologies z detektorem diodowym (DAD). Oznaczenia prowadzono w układzie faz odwróconych (faza ruchoma: metanol: roztwór kwasu octowego) z zastosowaniem kolumny Ultra C18 (250 x 4,6 mm o dp = 5 μm). Opracowana metoda oznaczania 2-metylo-4,6-dinitrofenolu polega na przepuszczeniu badanego powietrza przez rurkę szklaną wypełnioną żelem krzemionkowym. Próbki desorbowano metanolem i poddano analizie chromatograficznej (HPLC-DAD). Na podstawie wyników badań ustalono warunki oznaczania 2-metylo-4,6-dinitrofenolu w powietrzu na stanowiskach pracy w zakresie stężeń 0,005 ÷ 0,1 mg/m³. Walidację metody przeprowadzono zgodnie z wymaganiami zawartymi w normie europejskiej PN-EN 482. Uzyskano następujące dane walidacyjne: − zakres pomiarowy 0,005 ÷ 0,1 mg/m3 − granica wykrywalności, LOD 1,55 ng/ml − granica oznaczalności, LOQ 4,66 mg/ml, − całkowita precyzja badania 5,24 %, − względna niepewność całkowita 1,5 %. Opracowana metoda analityczna umożliwia selektywne oznaczanie 2-metylo-4,6-dinitrofenolu w powietrzu na stanowiskach pracy w zakresie stężeń od 0,005 mg/m3 (1/10 wartości NDS) w obecności substancji współwystępujących – fenoli i krezoli. Metoda charakteryzuje się dobrą precyzją i dokładnością, spełnia wymagania zawarte w normie europejskiej PN-EN 482 dla procedur dotyczących oznaczania czynników chemicznych. Opracowana metoda oznaczania 2-metylo-4,6-dinitrofenolu w powietrzu na stanowiskach pracy została zapisana w postaci procedury analitycznej, którą zamieszczono w załączniku.

EN

2-Methyl-4,6-dinitrophenol (DNOC) is a yellow crystalline solid. It has insecticidal, fungicidal and herbicidal properties. Nowadays, DNOC is used as a polymerization inhibitor and as an intermediate in the chemical industry. It is extremely toxic to humans.The aim of this study was to develop a new method for determining DNOC concentrations in workplace air in the range from 1/10 to 2 MAC values in accordance with the requirements of Standard No. EN 482.The study was performed using a liquid chromatograph (Agilent Technologies series 1200) with a diode array detector (DAD). The determination was performed in the reverse-phase system (mobile phase: methanol: solution of acetic acid) using an Ultra C18 column (250 × 4.6 mm with dp= 5 μm).The method was based on passing air through a silica gel tube. Samples were desorbed with methanol and analyzed with HPLC-DAD. The procedure was validated according to Standard No. EN 482. The measuring range was 0.005 ÷ 0,1 mg/m3, the limit of detection(LOD) was 1.55 ng/ml, the limit of quantification (LOQ) was 4.66 ng/ml, the overall accuracy of the method was 5.24% and the relative total uncertainty of the method was 11.5%.The analytical method described in this paper makes it possible to selectively determine DNOC in workplace air in the presence of phenols and cresols at concentrations from 0.005 mg/m³ (1/10 MAC value). The method is precise, accurate and it meets the criteria for procedures for measuring chemical agents listed in Standard No. EN 482. The developed method of determining DNOC has been recorded as an analytical procedure (see appendix).

14

Simultaneous determination of four major constituents in Citri Grandis Exocarpium by HPLC-DAD

Yu X. X., Liu Q. D., Wu J. W., Liang Z. K., Zhao M. Q., Xu X. J.

Acta Chromatographica

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2016

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Vol. 28, no. 1

129--143

EN

Citri Grandis Exocarpium (CGE) is a traditional Chinese medicine with a variety of biological activities. For efficient quality control of CGE, a simple, rapid, and accurate high-performance liquid chromatographic (HPLC) method was developed for simultaneous determination of four main compounds (naringin, rhoifolin, meranzin hydrate, and isoimperatorin) in this herb. These four compounds were separated on a C18 column by gradient elution with methanol and water. The flow rate was 1.0 mL•min−1, and the detection wavelength was 324 nm. The recoveries of the method ranged from 96.32% to 103.71%, and good linear relationships (r2 > 0.9998) over relative wide concentration ranges were obtained. Then this validated method was successfully applied to the analysis of nine batches of CGE samples.

15

Tiuram : oznaczanie w powietrzu na stanowiskach pracy

Dobrzyńska E., Woźnica A.

Podstawy i Metody Oceny Środowiska Pracy

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2015

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Nr 1 (83)

119--130

PL

Tiuram jest bezbarwną substancją: stałą, palną i nielotną o charakterystycznym zapachu, nierozpuszczalną w wodzie. Substancja znalazła zastosowanie w Polsce przede wszystkim w rolnictwie jako substancja aktywna chemicznych środków ochrony roślin (głównie fungicydów) oraz w przemyśle chemicznym jako, tzw. przyspieszacz procesów wulkanizacji w produkcji gumy. Tiuram jest stosowany również w medycynie i kosmetologii, jako filtr przeciwsłoneczny i środek przeciwgrzybiczny. Mechanizm toksycznego działania tiuramu jest wielokierunkowy. Głównymi objawami zatrucia substancją są: bóle głowy, nudności i wymioty, zaburzenia rytmu serca oraz trudności w oddychaniu. Często w następstwie zatrucia ostrego rozwija się: zapalenie spojówek, zapalenie oskrzeli, pokrzywka i wypryski skórne.

EN

Thiram is a colorless, combustible and non-volatile solid substance with a characteristic odor, practically insoluble in water. In Poland, thiram is used mainly as an agricultural chemical active ingredient of plant protection products (mainly fungicides) and as an accelerator in the chemical industry. In medicine or cosmetology, it is used as a sunscreen and antifungal agent. The mechanism of toxicity of thiram is multidirectional. The main symptoms of poisoning with thiram are headache, nausea and vomiting, heart rhythm disturbances, and difficulty in breathing. Often, as a result of acute poisoning conjunctivitis, bronchitis, urticaria and skin eruptions develop.

16

Efektywność fotodegradacji WWA w ściekach koksowniczych

Włodarczyk-Makuła M., Turek A., Obstój A

Ekologia i Technika

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2015

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R. 23, nr 6

354--359

PL

Celem pracy było określenie efektywności degrada ej i WWA w ściekach przemysłowych podczas działania promieniami ultrafioletowymi. Badania prowadzono z wykorzystaniem ścieków koksowniczych pobranych z odpływu zakładowej biologicznej oczyszczalni. Naświetlanie ścieków promieniami ultrafioletowymi prowadzono stosując zmienny czas ekspozycji: 30, 60 i 90 sekund. Stężenia WWA oznaczano w ściekach przed i po naświetlaniu metodą HPLC z detektorem fluorescencyjnym. Przygotowanie próbek do oznaczania ilościowego WWA polegało na wydzieleniu matrycy organicznej ze ścieków podczas ekstrakcji ciecz-ciecz z zastosowaniem mieszaniny rozpuszczalników organicznych: cykloheksanu i dichlorometanu. Oznaczano: naftalen Naf, acenaften Ac, fenantren Fen, antracen Ant, fluoren Flu, piren Pir, benzo(a)antracen BaA, chryzen Ch. Podczas ekspozycji ścieków na promieniowanie ultrafioletowe odnotowano obniżenie sumarycznego stężenia WWA do 31%. Efektywność usuwania poszczególnych WWA była różna: w zakresie od 4,6 do 66,9%.

EN

The results of investigations into the efficiency of PAHs removal from wastewater treated by ultraviolet rays are presented in this study. The investigations were carried out using wastewater originating from a industrial treatment plant. The samples of wastewater were exposed to UV rays for 30, 60 and 90 seconds After exposition to UV rays the PAHs concentration was determined in the wastewater samples. The extraction of organie matrix from samples was madę in the mixture of: cyclohexane and dichloromethane and methanol. The quantitative analysis of PAHs by HPLC with fluorescene detector was carried out. After exposition to ultraviolet rays decrease in PAHs concentration in the samples was observed. Exposure of wastewater to UV-rays resulted in a decrease in the concentration of PAHs In wastewater coming from a industrial wastewater treatment plant up to 31%. The efficiency of the removal of individual hydrocarbons was different and was in the range of 4,6 to 66,9%.

17

Validated Selective HPLC-DAD Method for the Simultaneous Determination of Diclofenac Sodium and Lidocaine Hydrochloride in Presence of Four of Their Related Substances and Potential Impurities

Belal T. S., Bedair M. M., Gazy A. A., Guirguis K. M.

Acta Chromatographica

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2015

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Vol. 27, no. 3

477--493

EN

This study presents a selective high-performance liquid chromatography (HPLC) with diode array detection (DAD) method for the simultaneous estimation of diclofenac sodium and lidocaine hydrochloride in presence of four of their related substances and potential impurities, namely, 2,6-dimethylaniline (DMA), 2,6-dichloroaniline (DCA), N-phenyl-2,6-dichloroaniline (PDCA), and N-chloroacetyl-N-phenyl-2,6-dichloroaniline (CPDCA). Some of these related substances are reported as degradation products as well. Effective chromatographic separation was achieved using Waters Symmetry C18 column, (3.9 × 150 mm, 5 μm particle size) with gradient elution of the mobile phase composed of 0.05 M orthophosphoric acid and acetonitrile. The gradient elution started with 5% (by volume) acetonitrile, ramped up linearly to 65% in 5 min then kept constant till the end of the run. The mobile phase was pumped at a flow rate of 1.5 mL min−1. The multiple wavelength detector was set at 220 nm, and quantification of both drugs was based on measuring their peak areas. The retention times for lidocaine and diclofenac were about 5.5 and 9.5 min, respectively. The reliability and analytical performance of the proposed HPLC procedure were statistically validated with respect to system suitability, linearity, ranges, precision, accuracy, specificity, robustness, detection, and quantification limits. Calibration curves were linear in the ranges of 10–200 μg mL−1 for both drugs with correlation coefficients not less than 0.9998. The proposed method proved to be selective by resolution of the two drugs from their related substances and potential impurities. The validated HPLC method was successfully applied to the analysis of this binary mixture in the combined formulation (ampoules dosage form), and the assay results were favorably compared with a previously reported HPLC method. The proposed method made use of DAD as a tool for peak identity and purity confirmation.

18

Bezwodnik octowy. Oznaczanie w powietrzu na stanowiskach pracy

Woźnica A., Kowalska J.

Podstawy i Metody Oceny Środowiska Pracy

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2014

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Nr 4 (82)

129--142

PL

W artykule przedstawiono metodę oznaczania bezwodnika octowego w powietrzu na stanowiskach pracy z zastosowaniem wysokosprawnej chromatografii cieczowej (HPLC) z detektorem diodowym (DAD).Metoda polega na: adsorpcji bezwodnika octowego na filtry z włókna szklanego z naniesioną 3,4- dimetoksybenzyloaminą i ftalanem dioktylu, ekstrakcji utworzonej pochodnej roztworem amoniaku i analizie chromatograficznej otrzymanego roztworu. Analizę prowadzono w układzie faz odwróconych (faza ruchoma: acetonitryl: kwas fosforowy) z zastosowaniem kolumny Ultra Cis.Zakres pomiarowy wynosi 1,2 - 24 mg/m3 dla próbki powietrza o objętości 7,5 1. Granica wykrywalności (LOD) metody wynosi 3,1 ng/ml, natomiast granica oznaczalności (LOQ) 9,3 ng/ml. Opracowaną metodę oznaczania bezwodnika octowego zapisano w' postaci procedury analitycznej, którą zamieszczono w Załączniku.

EN

This method describes how to measure acetic anhydride in workplace air using high- performance liquid chromatography (HPLC) with a diode array detector (DAD). Samples are collected onto glass fiber filters coated with 3,4-di- methoxybenzylamine and di-n-octyl phthalate. Samples are extracted with aqueous ammonium hydroxide and analysed with HPLC. The determination was carried out in the reverse-phase system (mobile phase: acetonitrile : phosphoric acid) using an Ultra C18 column. The measurement range was 1.2-24 mg/m3 for a 7.5-L air sample. Limit of detection (LOD): 3.1 ng/ml; limit of quantification (LOQ): 9.3 ng/ml. The developed method of determining acetic anhydride has been recorded as an analytical procedure, which is available in the Appendix.

19

Simultaneous determination of gallic acid, protocatechuic acid, catechin, epicatechin, quercetin and kaempferol in Chinese chestnut (Castanea mollissima blume) kernel by high-performance liquid chromatography with diode array detection

Wang T., Yang Y. D., Du B., Yu S., Hou W. L.

Acta Chromatographica

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2014

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Vol. 26, no. 3

539--550

EN

Chestnut exhibits anti-inflammatory, styptic, anti-diarrhea, and analgestic effects as a traditional Chinese medicine. There is increasing evidence that shows that the consumption of chestnuts has become more important in human nutrition due to the health benefits provided by the antioxidants. The phenolic compounds are responsible for major bioactivities, such as anti-tumor and anti-oxidation. A high-performance liquid chromatography (HPLC) method with diode array detection (DAD) was established for the simultaneous determination of six phenolic compounds (gallic acid, GA; protocatechuic acid, PR; catechin, CA; epicatechin, EP; quercetin, QU; kaempferol, KA) in Chinese chestnut (Castanea mollissima blume) kernel. The sample followed by separation on Eclipse XDB-C18 column (150 × 4.6 mm, id., 5 μm) with gradient elution of methanol-1.0% acetate acid solution as a mobile phase, at a temperature of 30°C, under the ratio of 1.2 mL min-1, with 5 μL injection volume, and multi-wavelength synthesis was used with DAD. The correlation coefficients were larger than 0.999, the recoveries were 97.58% for GA, 100.41% for PA, 96.23% for CA, 101.38% for QU, 99.15% for EP, and 98.60% for KA, relative standard deviation (RSD) were 1.04% for GA, 1.21% for PA, 1.09% for CA, 1.19% for QU, 1.06% for EP, and 1.20% for KA. This method was applied for the determination of phenolics in chestnut kernel and was found to be fast, sensitive, and suitable.

20

Multiple compounds determination and fingerprint analysis of Agrimonia pilosa Ledeb by high-performance liquid chromatography

Wang Y., Yin L., Lv G., Xu Y., Xu L., Qi Y., Zheng L., Peng J.

Acta Chromatographica

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2014

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Vol. 26, no. 1

137--156

EN

In the present paper, a simple and reliable high-performance liquid chromatography-diode array detection (HPLC-DAD) method was developed both for quantitative determination and fingerprint analysis of Agrimonia pilosa Ledeb for quality control. Under the optimized HPLC conditions, seven bioactive compounds including rutin, quercetin-3-rhamnoside, luteoloside, tiliroside, apigenin, kaempferol, and agrimonolide were determined simultaneously. For fingerprint analysis, 11 common peaks were selected as the characteristic peaks to evaluate the similarities of 16 different samples collected from different origins in China. Besides, hierarchical cluster analysis (HCA) was also performed to evaluate the variation of the raw materials. This is the first report of using a simple method for quality control of A. pilosa Ledeb through multi-component determination and chromatographic fingerprint analysis to the best of our knowledge.