scholarly journals Development of TLC Chromatographic-Densitometric Procedure for Qualitative and Quantitative Analysis of Ceftobiprole

Processes ◽  
2021 ◽  
Vol 9 (4) ◽  
pp. 708
Author(s):  
Żaneta Binert-Kusztal ◽  
Małgorzata Starek ◽  
Joanna Żandarek ◽  
Monika Dąbrowska
Keyword(s):  
High Sensitivity ◽  
Biologically Active ◽  
Fifth Generation ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Lipophilicity Parameter ◽  
Alkaline Environments ◽  
Acetic Acid Water ◽  
Cephalosporin Antibiotics ◽  
The Stability

Currently, there is still a need for broad-spectrum antibiotics. The new cephalosporin antibiotics include, among others, ceftobiprole, a fifth-generation gram-positive cephalosporin, active against Staphylococcus aureus methicillin agonist (MRSA). The main focus of the work was to optimize the conditions of ceftobiprole qualitative determination and to validate the developed procedure according to ICH guidelines. As a result of the optimization process, HPTLC Cellulose chromatographic plates as a stationary phase and a mixture consisting of ethanol:2-propanol: glacial acetic acid: water (4:4:1:3, v/v/v/v) as a mobile phase were chosen. The densitometric detection was carried out at maximum absorbance of ceftobiprole (λ = 232 nm). Next, the validation process of the developed procedure was carried out. The relative standard deviation (RSD) for precision was less than 1.65%, which proves the high compatibility of the results, as well as the LOD = 0.0257 µg/spot and LOQ = 0.0779 µg/spot values, which also confirm the high sensitivity of the procedure. The usefulness of the developed method for the stability studies of ceftobiprole was analyzed. Study was carried out under stress conditions, i.e., acid and alkaline environments, exposure to radiation imitating sunlight and high temperature (40–60 °C). It was found that cefotbiprole is unstable in an alkaline environment and during exposure to UV-VIS radiation. Moreover, the lipophilicity parameter, as a main physicochemical property of the biologically active compound, was determined using experimental and computational methods.

scholarly journals Validation of the alkalimetry method for the quantitative determination of free organic acids in raspberry leaves

2021 ◽  
Vol 19 (1(73)) ◽  
pp. 53-58
Author(s):  
O. Yu. Maslov ◽  
S. V. Kolisnyk ◽  
T. A. Kostina ◽  
Z. V. Shovkova ◽  
E. Yu. Ahmedov ◽  
...  
Keyword(s):  
Organic Acids ◽  
Quantitative Determination ◽  
Biologically Active ◽  
Intermediate Precision ◽  
Potentiometric Detection ◽  
Class A ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Intermediate Metabolites

 Organic acids are a large group of biologically active compounds that perform important functions in the plant organism. Moreover, all plants, regardless of the species and family, contain organic acids to a small or large extent as organic acids belong to intermediate metabolites arising from the oxidation of proteins and amino acids, fats and carbohydrates.Aim. To validate the method of alkalimetry proposed with potentiometric detection of the end-point for the quantitative determination of free organic acids in raspberry leaves.Results and discussion. The method proposed was validated according to the International Conference on Harmonization (ICH) guidelines. The linearity was in the concentration range of 40 – 200 % (r2 = 0.9991). The percentage of recovery was found to be in the range of 98.77 – 102.48 %. The repeatability and intermediate precision were 1.58 % and 1.74 %, respectively. The method is accurate and reliable, with the relative standard deviation of less than 2 %.Experimental part. Leaves of raspberry were collected in the Kharkiv region during the period of full ripening. A Hanna 2550 pH-meter with a HI 1131P potentiometric electrode was used for alkalimetric titration of free organic acids. The titration was carried out using a microburette with Class A accuracy.Conclusions. The alkalimetry method for the quantitative determination of free organic acids in raspberry leaves has been proposed and validated according to the following parameters: specifcity, linearity, accuracy, repeatability, intermediate precision, robustness. It has been confrmed that the method is simple, reliable, accurate and cost-effective.Key words: raspberry; leaves; free organic acids; alkalimetry; validation

Atomic absorption determination of Hg (II), Cd (II), and As (III) in natural and waste water after preliminary group preconcentration

2019 ◽  
Vol 85 (2) ◽  
pp. 12-16
Author(s):  
I. V. Saunina ◽  
E. N. Gribanov ◽  
E. R. Oskotskaya
Keyword(s):  
Waste Water ◽  
Atomic Absorption ◽  
High Sensitivity ◽  
Distribution Coefficients ◽  
Neutral Medium ◽  
Atomic Absorption Determination ◽  
Absorption Determination ◽  
Relative Standard ◽  
Preliminary Group

The sorption of Hg (II), Cd (II), and As (III) by natural aluminosilicate is studied. It is shown that the mineral absorbs those toxicants in a rather wide pH range, quantitative extraction of analytes being achieved in a neutral or close to neutral medium (pH values range within 7.0 - 8.0; 6.3 - 7.5; 7.4 - 8.5 for Hg (II), As (III), and Cd (II), respectively). The effect of the time of phase contact on the degree of extraction of elements is shown. The sorption capacity of the mineral in optimal conditions of the medium acidity (0.06 mmol/g for mercury, 0.31 mmol/g for cadmium, and 0.52 mmol/g for arsenic) is determined. The distribution coefficients attain values of aboutnX 103-nX 104. A new combined method for determination of Hg (II), Cd (II), and As (III) in natural and waste water is developed and tested. The method consists in a preliminary group sorption concentration of the analytes by aluminosilicate, desorption of the analytes from the surface of the mineral and their subsequent atomic absorption determination. The correctness of the method is verified in analysis of spiked samples. The method is easy to use and exhibits high sensitivity, reproducibility and accuracy of analyte determination. The relative standard deviation does not exceed 0.13. Economic availability and possibility of using domestic sorption materials are the important advantages of the proposed procedure which can be used in the practice of laboratories monitoring the quality and safety of environmental objects.

scholarly journals Quantitative analysis of doxorubicin hydrochloride and arterolane maleate by mid IR spectroscopy using transmission and reflectance modes

BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Ranju Bansal ◽  
Ranjit Singh ◽  
Khushpal Kaur
Keyword(s):  
Quantitative Analysis ◽  
Spectroscopic Methods ◽  
Doxorubicin Hydrochloride ◽  
Intermediate Precision ◽  
Solid Dosage ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Ft Ir ◽  
Solid Bulk ◽  
Ir Spectroscopic

Abstract Background Environment-friendly fast and accurate mid-infrared spectroscopic methods have been developed for the quantitative analysis of doxorubicin hydrochloride (DOX) and arterolane maleate (ALM) in bulk and marketed formulations. Both transmittance and reflectance modes have been used for the analysis and a comparison has been drawn for better accuracy. The analytical methods were validated in accordance with International Council for Harmonisation (ICH) guidelines Results The proposed methods have been successfully developed and validated for the quantification of doxorubicin and arterolane maleate in solid bulk and dosage form. High recovery values in both the modes, while analysing DOX and ALM, indicated good accuracy of the methods. The methods showed excellent repeatability and intermediate precision [% RSD (Relative Standard Deviation < 2.0%]. The assay values of the drugs in solid dosage forms were also found close to the labelled claim. Conclusion The proposed Fourier transform infrared (FT-IR) spectroscopic methods were found to be specific, reproducible, valid and could be used as general methods for the quantification of most of the solid drug preparations such as tablets, capsules and powders.

Chromogranin a Measurement in Neuroendocrine Tumors

1998 ◽  
Vol 13 (1) ◽  
pp. 3-9 ◽  
Author(s):  
L. Ferrari ◽  
E. Seregni ◽  
A. Martinetti ◽  
B Van Graafeiland ◽  
S. Nerini-Molteni ◽  
...  
Keyword(s):  
Tumor Marker ◽  
Neuroendocrine Tumors ◽  
Chromogranin A ◽  
High Sensitivity ◽  
Biologically Active ◽  
Proliferative Index ◽  
Favorable Prognosis ◽  
Blood Marker ◽  
Active Substances

Neuroendocrine tumors (NETs) are rare neoplasms characterized by a low proliferative index and, in some cases, a favorable prognosis. These tumors often overproduce and release biologically active substances that are responsible for severe syndromes. Tumor marker measurement provides the clinician with useful information for the management of NET patients. The substances released by overproducing tumors are currently used as biomarkers, but there is a need for sensitive markers also for the “biochemically silent” NETs. The most effective and reliable blood marker available today is chromogranin A (CgA). Because of its high sensitivity and specificity, this glycoprotein can be used for the diagnosis, prognosis and follow-up of NETs. Furthermore, CgA measurement can be used for monitoring those tumors not overproducing or releasing any hormones or biological amines. This paper is a synthetic review on the value of CgA in NET management and reports our experiences with CgA measurement in NET patients.

scholarly journals Nucleic-Acid-Binding Chromophores as Efficient Indicators of Aptamer-Target Interactions

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Kwabena Sarpong ◽  
Bhaskar Datta
Keyword(s):  
Nucleic Acid ◽  
High Sensitivity ◽  
Covalent Modification ◽  
Fluorescence Signal ◽  
Nucleic Acid Binding ◽  
Sensitivity And Selectivity ◽  
Target Molecules ◽  
Diagnostic Applications ◽  
The Stability ◽  
Simple Format

The binding affinity and specificity of nucleic acid aptamers have made them valuable candidates for use as sensors in diagnostic applications. In particular, chromophore-functionalized aptamers offer a relatively simple format for detection and quantification of target molecules. We describe the use of nucleic-acid-staining reagents as an effective tool for detecting and signaling aptamer-target interactions. Aptamers varying in size and structure and targeting a range of molecules have been used in conjunction with commercially available chromophores to indicate and quantify the presence of cognate targets with high sensitivity and selectivity. Our assay precludes the covalent modification of nucleic acids and relies on the differential fluorescence signal of chromophores when complexed with aptamers with or without their cognate target. We also evaluate factors that are critical for the stability of the complex between the aptamer and chromophore in presence or absence of target molecules. Our results indicate the possibility of controlling those factors to enhance the sensitivity of target detection by the aptamers used in such assays.

scholarly journals Analysis of Mercury in Skin Lightening Cream by Microwave Plasma Atomic Emission Spectroscopy (MP-AES)

Molecules ◽  
2021 ◽  
Vol 26 (11) ◽  
pp. 3130
Author(s):  
Hardoko I. Qudus ◽  
Purwadi Purwadi ◽  
Iis Holilah ◽  
Sutopo Hadi
Keyword(s):  
Emission Spectroscopy ◽  
Microwave Plasma ◽  
Atomic Emission ◽  
Atomic Emission Spectroscopy ◽  
Solution Stability ◽  
Analysis Method ◽  
Plasma Atomic Emission ◽  
Relative Standard ◽  
The Stability ◽  
Skin Lightening

This research aimed at developing an analysis method, which was optimized and validated to determine the content of mercury in skin lightening cream discovered in the market in Bandar Lampung, Indonesia, through the use of microwave plasma atomic emission spectroscopy (MP-AES). The optimization on the analysis method was conducted on pump rate, viewing position, and reductant concentration in order to obtain the highest mercury emission intensity, while the solution stability was optimized to know the stability of mercury in the solution. The result showed that the method developed had precision with a relative standard deviation of 2.67%, recovery value of 92.78%, and linearity with an r value of 0.993, respectively. The sensitivity of the instrument detection had a limit of analysis method detection and quantification of 0.59 and 1.98 µg/L, respectively. The results of the test of the lightening cream (8 of 16 samples) positively contained mercury in the range of 422.61–44,960.79 ng/g. Therefore the method of analysis developed may be used for routine analysis of chemicals in any cosmetics products.

RP-HPLC METHOD DEVELOPMENT FOR THE ASSAY OF AMPHOTERICIN B

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (02) ◽  
pp. 16-20
Author(s):  
L Mohankrishna ◽  
◽  
P. J. Reddy ◽  
B. P Reddy. ◽  
P. Navya
Keyword(s):  
Amphotericin B ◽  
Mobile Phase ◽  
Method Development ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Phase Combination ◽  
Hplc Method Development

A sensitive and precise HPLC procedure has been developed for the assay of amphotericin B in bulk samples and pharmaceutical formulations by using a C18 column [Kromosil, C18, (5 µm, 4.6mm x 250 mm; Make. Waters)], and mobile phase combination is 1% formic acid in water and acetonitrile in ratio of 45:55 V/V. The procedure has been validated as per the ICH guidelines. The λmax of detection was fixed at 407 nm, so that there was less interference from mobile phase with highest sensitivity according to UV analysis. Calibration plots were linear in the range of 10-100 µg/mL and the LOD and LOQ were 0.02 µg/mL and 0.06 µg/mL respectively. The high recovery and low relative standard deviation confirm the suitability of the method for routine quality control determination of amphotericin B in different formulations.

scholarly journals Simultaneous determination of clobutinol hydrochloride and doxylamine succinate from syrups by RP HPLC using a new stationary phase containing embedded urea polar groups

2012 ◽  
Vol 48 (2) ◽  
pp. 315-323 ◽  
Author(s):  
Paulo Cesar Pires Rosa ◽  
Isabel Cristina Sales Fontes Jardim
Keyword(s):  
Stationary Phase ◽  
Simultaneous Determination ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Polar Groups ◽  
Ich Guidelines ◽  
Relative Standard ◽  
New Stationary Phase

A new, simple, fast, reproducible and sensitive reversed phase HPLC method, using a new stationary phase containing embedded urea polar groups, has been developed and validated for the simultaneous determination of clobutinol hydrochloride (CLO) and doxylamine succinate (DOX) in syrups. The determination was carried out on a C8 urea column (125 mm x 3.9 mm i.d., 5 µm particle size) synthetized at the Liquid Chomatography Laboratory (LabCrom) of the Chemistry Institute of Unicamp. The mobile phase consisted of a mixture of acetonitrile:methanol:phosphate buffer (pH 2.5) in the gradient mode. The diode array detector (DAD) was operated at 230 nm for CLO and 262 nm for DOX. The method showed adequate precision, with relative standard deviations (RSD) less than 1%. The presence of the excipients did not interfere in the results of the analysis. Accuracy was determined by adding standards of the drugs to a placebo and good recovery values were obtained. The analytical curves were linear (r² 0.9999 for CLO and 0.9998 for DOX) over a wide concentration range (2.4-336 µg mL-1 for CLO and 2.3-63 µg mL-1 for DOX). The solutions were stable for at least 72 hours at room temperature. The criteria for validation using the ICH guidelines were fulfilled.

Design of Photoionization Detector Based on the Miniature Gas Chromatography

2013 ◽  
Vol 823 ◽  
pp. 291-295 ◽  
Author(s):  
Shou Chen Chai ◽  
Peng Yang ◽  
Cheng Jia Yang ◽  
Chun Li Cai ◽  
Na Yu
Keyword(s):  
Gas Chromatography ◽  
Detection Limit ◽  
Ionization Chamber ◽  
High Sensitivity ◽  
Fast Response ◽  
Low Detection Limit ◽  
Photoionization Detector ◽  
Key Factor ◽  
The Stability ◽  
Sensitivity Detection

In the space restricted airtight environment that people lives in, detecting harmful gas by miniature gas chromatography is the practical requirement at present, however, PIDs performance is key factor that restrict the application of miniature gas chromatography, the redesign of the detectors gas route in this paper aiming at improve detectors stability observably, and schemed out miniature PID with high sensitivity, low detection limit and fast response. The result of the experiment shows that the detection limit is 0.04ppm, the sensitivity is 101mv/ppm,the stability is 0.04×10-6/24h,meeting the project requirement. Keywords: photoionization detector; ionization chamber; sensitivity; detection limit;

scholarly journals Simultaneous Rapid Detection of Aflatoxin B1 and Ochratoxin A in Spices Using Lateral Flow Immuno-Chromatographic Assay

Foods ◽  
2021 ◽  
Vol 10 (11) ◽  
pp. 2738
Author(s):  
Xue Zhao ◽  
Xindi Jin ◽  
Zhang Lin ◽  
Qi Guo ◽  
Bin Liu ◽  
...  
Keyword(s):  
Ochratoxin A ◽  
Aflatoxin B1 ◽  
High Performance ◽  
Simultaneous Detection ◽  
High Sensitivity ◽  
Strong Stability ◽  
Test Strip ◽  
Chromatography Analysis ◽  
Relative Standard ◽  
Strip Test

Spices are susceptible to contamination by aflatoxin B1 (AFB1) and ochratoxin A (OTA), which are both mycotoxins with high toxicity and carcinogenicity. In this study, we aimed to develop an immuno-chromatographic strip test for the simultaneous quantification of AFB1 and OTA in spices by spraying the coupled antigens AFB1–ovalbumin (AFB1–OVA) and OTA–ovalbumin (OTA–OVA) on a nitrocellulose membrane. The test strip had high sensitivity, good specificity, and strong stability. The detection limits of these two mycotoxins in Chinese prickly ash, pepper, chili, cinnamon, and aniseed were 5 μg/kg. The false positivity rate was 2%, and the false negativity rate was 0%. The maximum coefficient of variation was 4.28% between batches and 5.72% within batches. The average recovery rates of AFB1 and OTA in spices were 81.2–113.7% and 82.2–118.6%, respectively, and the relative standard deviation (RSD) was <10%. The actual sample detection was consistent with high performance liquid chromatography analysis results. Therefore, the immuno-chromatographic test strips developed in this study can be used for the on-site simultaneous detection of AFB1 and OTA in spices. This method would allow the relevant regulatory agencies to strengthen supervision in an effort to reduce the possible human health hazards of such contaminated spices.

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