Journal of Chemical Metrology

Articles In Press

Original Article

1) Determination of secondary metabolites of Origanum vulgare subsp. hirtum and O. vulgare subsp. vulgare by LC-MS/MS

J. Chem. Metrol. (2020) in press ; 1 - 10
by Züleyha Özer , Sema Çarıkçı , Hasibe Yılmaz , Turgut Kılıç , Tuncay Dirmenci and Ahmet C. Gören

Secondary metabolites of solvent extracts of Origanum vulgare subsp. hirtum and O. vulgare subsp. vulgare were determined using liquid chromatography–mass spectrometry (LC-MS/MS). Curcumin was used as an internal standard. Rosmarinic acid was determined as the main compound of studied extracts together with other phenolic acid derivatives.  In LC-MS/MS analyses, relative standard deviations (RSD %) ranged between 0.11-9.47. The correlation values were found to be greater than 0.97 for each investigated analyte.

DOI
http://doi.org/10.25135/jcm.33.20.04.1610
(DOI number will be activated after the manuscript has been available in an issue.)
Keywords
Origanum phenolic compounds LC-MS/MS method validation uncertainty assessment rosmarinic acid
Available online: May 09, 2020
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Original Article

2) Rapid and easy method for simultaneous measurement of widespread 27 compounds in natural products and foods

J. Chem. Metrol. (2020) in press ; 1 - 11
by Özge Tokul-Ölmez , Bihter Sahin , Cansel Çakır and Mehmet Ozturk

Phenolic compounds are dietary bioactive compounds that are available in foods and beverages. They are produced by the plant and/or by the mushrooms, naturally. Some of the natural phenolic compounds were also used in dietary supplements in the pharmaceutical or food industries. For simultaneous analyses of phenolic compounds in one injection, a rapid and sensitive method was developed for twenty-seven natural compounds using reverse-phase high-performance liquid chromatography (RP-HPLC) coupled with diode array detector (DAD). The linear gradient elution systems of 0.1% acetic acid-methanol were used, and the analyzing time was 61 minutes. The method was validated with linearity, relative error, reproducibility, LOD values. Relative standard deviation between (n = 7) within and between days for reproducibility is less than 10%, and relative error (or recovery) is less than 5%. The method exhibited excellent linearity (R2>0.999), good precision (RSD<6.1%), recovery (97.6–104.1%) and limits of detection (0.23–28.81 µg/m1) and quantification (1.62– 87.29 µg/m1). The detection of compounds was performed at 220 nm, 280 nm, and 330 nm. The developed method for the rapid determination of phenolic compounds using RP-HPLC can be used to identify the availability of these phenolic compounds in natural and commercial products.

DOI
http://doi.org/10.25135/jcm.38.20.03.1589
(DOI number will be activated after the manuscript has been available in an issue.)
Keywords
RP-HPLC phenolic compounds food dietary supplements natural products
Available online: May 02, 2020
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Original Article

3) Importance of sample pretreatment step on the bacterial toxicity bioassay of ZnO nanoparticles

J. Chem. Metrol. (2020) in press ; 1 - 13
by Aslı Baysal , Hasan Saygin and Gul S Ustabasi

(Eco)toxicological assessment of engineered nanoparticles has largely restricted to laboratory conditions, and contribution to the environmental matrix mostly ignored. Thus, the lack of reflection of the environmental matrix makes it harder to evaluate the ecotoxicity of nanoparticles and its mechanism. Therefore, sample pretreatment has a vital role for appropriate (eco)toxicological assessment and reflection of the environmental matrix. The present study aims to investigate the effect of different sample pretreatment strategies on the (eco)toxicity of ZnO nanoparticles and its mechanism. For this purpose, three sample pretreatments and related bacterial bioassay procedure was examined. Moreover, the impact of the sample pretreatment on the toxicity mechanism was investigated using the physicochemical parameters of ZnO nanoparticles and antioxidant responses of bacteria. The results showed that the sample pretreatment affected the physicochemical properties of ZnO nanoparticles, inhibition level and inhibition pathway.

DOI
http://doi.org/10.25135/jcm.37.20.03.1583
(DOI number will be activated after the manuscript has been available in an issue.)
Keywords
Sample preparation nanoparticles bacterial bioassay matrix effect seawater
Available online: May 02, 2020
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Short Report

4) Determination of dihydrocapsaicin adulteration in dietary supplements using LC-MS/MS

J. Chem. Metrol. (2020) in press ; 1 - 6
by Demet Dincel , Hatice Olgan , Zeynep Canbaloglu , Sule Yalcin , Aysen Erkucuk , Gizem Tiris and Ahmet C. Gören

Adulteration of dietary supplements are serious threats to public health in all around of world. Nowadays, in order to obtain the intended effect from natural remedies, the adulteration of natural products via artificial or harmful chemicals are increasing. A rapid LC-MS/MS method for determination of capsaicin and dihydrocapsaicin in dietary supplements via Fortis C18 (150 x 3 mm; 3 µm) column at 25 °C was developed and validated in a mixture of mobile phase A (1 % formic acid solution and 0.1 % ammonium formate in water) and B (1 % formic acid solution and 0.1 % ammonium formate in methanol) with gradient program at a flow rate of 0.35 mL/min.  The recoveries of developed methods weytre obtained in the range of % 95.4-106.3 for capsaicin and % 96.3-108.9 for dihydrocapsaicin. This study shows that synthetic compound dihydrocapsaicin is widely use in dietary supplements products for adulteration to increase the effects of product without any declaration.  

DOI
http://doi.org/10.25135/jcm.36.20.01.1532
(DOI number will be activated after the manuscript has been available in an issue.)
Keywords
Capsaicin dihydrocapsaicin LC-MS/MS adulteration lose weight dietary supplements
Available online: April 19, 2020
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Original Article

5) Primary level electrolytic conductivity measurements at National Metrology Institute of Turkey (TUBITAK UME)

J. Chem. Metrol. (2020) in press ; 1 - 10
by Emrah Uysal , Lokman Liv , Fehmi Fıçıcıoğlu and Mehedin Arifoviç

TUBITAK UME (National Metrology Institute of Turkey) Electrochemistry Laboratory established the primary level electrolytic conductivity measurement system in 2018. The objective of this work is to prove the accuracy of the established system with an acceptable uncertainty and to disseminate the traceability for electrolytic conductivity measurements. While the accuracy of the system was tested with the certified conductivity solutions, the accuracy of the software developed at TUBITAK UME was also tested. The cell constant was determined as 0.57986 cm-1 at 25 °C by using certified conductivity solutions. The accuracy of the system was evaluated using the measurement of certified conductivity solutions and it was found that there was no significant difference between the results at 95% confidence level. Finally, “Evaluation of measurement data - Guide to the expression of uncertainty in measurement” and “EA-4/02 M: 2013 Evaluation of the Uncertainty of Measurement in Calibration” guides were used to form the uncertainty budget for primary level electrolytic conductivity measurements.

DOI
http://doi.org/10.25135/jcm.34.20.01.1524
(DOI number will be activated after the manuscript has been available in an issue.)
Keywords
Electrolytic conductivity jones cell CRM traceability
Available online: March 24, 2020
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Original Article

6) Liquid chromatographic analysis for the determination of deferasirox in pharmaceutical formulations and spiked plasma samples using dansyl chloride reagent

J. Chem. Metrol. (2020) in press ; 1 - 7
by Ali Asram Sagiroglu , Cem Onal and S. Evrim Kepekçi Tekkeli

In the current study, a new sensitive and precise method based on HPLC and derivatization with dansyl chloride was developed for quantification of deferasirox (DEF) in pharmaceutical dosage forms and spiked plasma samples. Separation procedure in the chromatographic system was performed using a mobile phase consisting of the mixture of methanol and acetic acid solution (0.5 M, pH adjusted to 7.0 with NaOH) with a ratio of 70:30 v/v at flow rate of 1.0 mL per minute under isocratic elution on a C18 column (150 mm × 4.6 mm, 5 μm I.D.). The excitation wavelength was selected as 340 nm and emission wavelength was selected as 480 nm for the measurement of the analyte signal. The retention time for DEF is approximately 3.5 min. ICH Guidelines were taken into account for method validation. For the deferasirox concentration range of 20–2000 ng/mL, the proposed analytical method exhibited a linear relationship between the drug concentration and measured fluorescence with a correlation coefficient of 0.9994.The currently developed method can be implemented efficiently for the quantification of DEF in pharmaceutical dosage forms and spiked plasma samples.

DOI
http://doi.org/10.25135/jcm.35.20.01.1518
(DOI number will be activated after the manuscript has been available in an issue.)
Keywords
Deferasirox HPLC method validation pharmaceutical formulation spiked plasma
Available online: March 24, 2020
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