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1

Chromatographic fingerprints and quantitative analysis for the quality evaluation of Bao-Yuan Decoction by ultra-performance liquid chromatography coupled with diode array and evaporative light scattering detection

Zhang Min, Zhu Zhenling, Wang Mengyue, Hou Jincai, Li Yinqing, Xiaobo Li

Acta Chromatographica

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2022

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Vol. 34, no. 1

87--99

EN

Bao-Yuan Decoction (BYD), a widely used traditional Chinese medicine formula, is worth developing into modern dosage forms. To assess the quality of traditional decoction, the commonly used ultra-performance liquid chromatography coupled with diode array and evaporative light scattering detection (UPLC-DAD/ELSD) method was initially applied to develop the analytical methods for the qualitative fingerprints and simultaneous quantitation of multiple marker compounds in BYD. Based on 16 batches of BYD prepared from multiple batches of qualified crude herbs combined randomly, the characteristic fingerprints were generated, with 41 and 19 common peaks detected by DAD and ELSD, respectively. Furthermore, ginsenosides Re, Rg1 and Rb1, calycosin-7-glucoside, calycosin, liquiritin, isoliquiritin apioside, isoliquiritin, glycyrrhizic acid and cinnamic acid were qualified as marker compounds to represent the herbs composing the formula. The characteristic fingerprints and the content ranges of multiple batches of the decoction were obtained, thus providing guidance for the quality control of modern dosage forms. The combination of these qualitative and quantitative methods will be an effective operational measure by which to evaluate and control the quality of BYD from traditional decoction to modern dosage forms.

2

Determination of the fatty acids in fish tissue and feed — comparison of different methods and statistical evaluation

Trbović D., Polak T., Demšar L., Parunović N., Dimitrijević M., Nikolić D., Đorđević V.

Acta Chromatographica

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2018

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Vol. 30, no. 3

175--179

EN

With the aim to reinforce laboratory competence in the field of testing the quality of fish from aquaculture, a study on the precision of fatty acid (FA) analyses in fish meat and fish feed was undertaken. Different methods were performed in laboratories. In situ transesterification method and extraction of lipids from the fish were followed by capillary gas chromatography with flame ionization detection. The reproducibility (R) values of the majority of FAs were less than 3% of their absolute values. Differences in calculating ionization detector response factors and/or autoxidation caused by faulty sample-handling could lead to variation in quantification of FAs in fish, especially for FA C22:6n-3. Statistical analysis showed a significant correlation between the two laboratories' quantifications of FAs in fish and fish feed (Pearson's correlation coefficient; r = 0.987, r = 0.994, and r = 0.997; for fish Z [trout], fish Š [rainbow trout], and fish feed, respectively). Overall, adequate accuracy was obtained in this study. The proposed method provides a fast and efficient means of identifying fish and feed for quality control purposes.

3

Quantitation of polyhexamethylene biguanide by photometric titration with Naphthol Blue Black dye

Ziółkowska D., Syrotynska I., Shyichuk A.

Polimery

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2014

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T. 59, nr 2

160--164

EN

A convenient and reliable method for quantitative determination of polyhexamethylene biguanide in aqueous solutions has been developed, based on complexation of the polymer with Naphthol Blue Black dye. Spectrophotometric titration measuring absorbance at 600 nm leads to characteristic zigzag curves, with the inflexion point at dye to polymer mers molar ratio 1:2. The photometric titration endpoints are characterized with good repeatability, resulting in low variance values. As a result, the limit of polyhexamethylene biguanide determination has been found to be equal to 50 and 150 µmol/dm3 of mers for direct and reverse titration, respectively.

PL

Opracowano nieskomplikowaną, dokładną metodę ilościowego oznaczania biguanidu poliheksametylenowego w roztworach wodnych opartą na reakcji kompleksowania polimeru z barwnikiem Czerń Amidowa 10B. Zmiany widma UV-Vis sugerują, że przy pewnym stosunku molowym stężeń polimeru (w przeliczeniu na mer) i barwnika tworzą się słabo rozpuszczalne kompleksy. Wynikiem miareczkowania spektrofotometrycznego przy długości fali 600 nm są zygzakowate zależności absorbancji od ilości analitu z punktem przegięcia przy stosunku molowym barwnik:polimer wynoszącym 1:2. Zastosowana metoda wyznaczania punktu końcowego miareczkowania charakteryzuje się dobrą powtarzalnością. Zakres oznaczania merów biguanidu poliheksametylenowego wynosi 50 i 150 µmol/dm3, odpowiednio, dla miareczkowania prostego i odwrotnego.

4

Quantitation of poly(diallyldimethylammonium chloride) by complexation with acid orange 7 dye

Ziółkowska D., Szeflińska I., Shyichuk A.

Polimery

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2014

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T. 59, nr 11-12

859--861

EN

The anionic dye Acid Orange 7 (AO7) was applied for quantitative determination of poly(diallyldimethylammonium chloride) (PDDA) in aqueous solutions. The PDDA polymer forms colloidal complexes with the AO7 dye resulting in spectral changes. Increase in the polymer concentration up to 0.10 mmol(mer)/dm3 leads to decrease in absorbance at wavelengths in the range between 450 and 500 nm. The obtained calibration dependences between absorbance and concentration fulfill linear equation with quite small variance (s2 = 1.56 · 10-2). The proposed method of PDDA quantitation requires weak acidic medium (pH » 3.5-6.5) and low values of ionic strength (I » 20 mM).

PL

Zdolność barwnika — oranżu kwasowego II (AO7) do tworzenia koloidalnych kompleksów z poli(chlorkiem dimetylodialliloamonowym) (PDDA) została wykorzystana do ilościowej analizy tego polimeru w roztworach wodnych. Wykazano, że oznaczenie stężenia PDDA za pomocą pomiaru absorbancji z wykorzystaniem krzywej wzorcowej jest możliwe w zakresie długości fali od 450 do 500 nm. Wzrostowi stężenia polimeru do 0,10 mmol(mer)/dm3 towarzyszy spadek intensywności głównego piku w widmie barwnika AO7, przy czym krzywa kalibracyjna ma charakter prostoliniowy. Zaproponowana metoda oznaczania PDDA wymaga zastosowania środowiska słabo kwasowego (pH » 3,5—6,5) i o małych wartościach siły jonowej (I » 20 mM).

5

HPLC analysis in drug level monitoring of K027

Nurulain S. M., Kalász H., Szegi P., Kuca K., Adem A., Hasan M. Y. B., Hashemi F., Tekes K.

Acta Chromatographica

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2013

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Vol. 25, no. 4

703--710

EN

HPLC monitoring of pharmacokinetics was done in two body compartments of rats following intramuscular treatments with three different doses of K027, a bispyridinium mono-aldoxime type of antidotes to organoposphate intoxicated subjects. Reversed-phase HPLC separation with electrochemical detections was done to monitor the onset, the maximum level, and offset in K027 concentration. Serum level of K027 showed a fast onset, independently from the doses of K027. Drug level in brain was showing an essentially delayed kinetics.

6

Development and validation of a TLC-densitometric method for the simultaneous quantitation of icariin and L-arginine from commercial formulations

Gupta P. K, Kuber V. V, Ghosh V. K, Bhope S. G, Sharma V., Purohit S

Acta Chromatographica

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2011

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Vol. 23, no. 3

447--458

EN

A simple, rapid, and specific thin layer chromatographic (TLC) method has been developed and validated for the simultaneous estimation of icariin and L-arginine from commercial polyherbal formulations for sexual dysfunction. The separation of the methanol extract of these formulations was achieved on silica gel 60 F254 aluminum backed TLC plates by using ethyl acetate-acetone-glacial acetic acid-formic acid-water 12:2:1:2:2 (υ/υ) as mobile phase. Densitometric analysis of icariin and L-arginine was monitored in absorbance mode at 270 and 195 nm, respectively. The linear regression analysis data for the calibration plots for icariin and L-arginine showed good linear relationship with r2 = 0.9984 +- 0.01 and 0.9968 +- 0.02, in the concentration ranges of 250–750 and 500–1500 ng/spot, respectively. The method was validated for precision, robustness, and recovery. The average percentage recovery was found to be 98.26% for icariin and 99.63% for L-arginine. The limits of detection and quantitation were 72, 116 and 238, 383 ng/spot, respectively, for icariin and L-arginine. Statistical analysis proves that the method is repeatable and selective for the estimation of the targeted drugs. Since the proposed mobile phase effectively resolves the icariin and L-arginine, this method can be applied for the identification and quantitation of these components in herbal extracts and marketed formulations.

7

Optimization of extraction of pyrrolizidine alkaloids from plant material

Mroczek T., Widelski J., Głowniak K.

Chemia Analityczna

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2006

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Vol. 51, No. 4

567-580

EN

Various techniques of extraction of pyrrol izidine alkaloids (PAs) from comfrey have been developed and compared. Different extraction media: methanol, ethanol, 1% methanolic solution of tartaric acid, 2.5% HC1 solution, 5% CH.COOH solution, alkaline chloro form- -methanol mixture at various temperatures (room temperature, 50-60°C, solvent's boiling point) have been used in various extraction techniques (percolation, electric basket, ultrasonic water bath) and various extraction times. Total concentration of pyrrolizidine alkaloids (PAs) was estimated from UV-VIS spectrophotometric studies according to Dann- -Mattocks procedure. For the most promising extraction techniques one determined recoveries of monocrotaline added to crude pre-extracts. Extraction and co-extraction processes were investigated using UV-VIS spectra of the adducts of 3,4-dehydro-PAs and Ehrlich's reagent. The best result of PAs extraction from comfrey was obtained using 1% methanolic solution of tartaric acid and electric basket technique at the temperature 100 š 5°C for 2 h. Possible applications of the method have been discussed.

PL

W prezentowanej pracy podjęto badania optymalizacji ekstrakcji alkaloidów pirolizydy-nowych (PAs) z materiału roślinnego (źywokostu lekarskiego). Zastosowane metody obejmowały ekstrakcję metanolem, etanolem, l % roztworem kwasu winowego w metanolu, 2.5% roztworem kwasu solnego, 5% roztworem kwasu octowego, alkaliczną fazą organiczną (chloroform-metanol). Badano również wpływ temperatury ekstrakcji (pokojowa, 50-60°C, wrzący rozpuszczalnik) wykorzystując różne techniki ekstrakcyjne (perkolacja, ekstrakcja w płaszczach grzewczych, ekstrakcja wspomagana ultradźwiękami) oraz wpływ czasu ekstrakcji na odzysk PAs z surowca roślinnego. Caikowitą zawartość PAs oznaczono w oparciu o spektrofotometrię UV-VIS wg metody Danna i Mattocksa. W przypadku najbardziej obiecujących metod ekstrakcji oznaczono odzysk wzorca monokrotaliny dodawanego do pre-ekstraktu tuż przed rozpoczęciem właściwej ekstrakcji. Analizując widma U V—VIS adduktów 3,4-dehydro-PAs z odczynnikiem Ehrlicha możliwa była analiza stopnia ekstrakcji PAs z surowcajak i współekstrakcji substancji balastowych. Najlepszą wydajnością oraz najmniejszym stopniem współekstrakcji balastów charakteryzowała się 2-godzinna ekstrakcja wrzącym (temp. 100 š 5°C) 1% roztworem kwasu winowego w metanolu w płaszczach grzewczych. Przedyskutowano także potencjalne wykorzystanie opracowanej metody.