scholarly journals Evaluation of analytical method for determination of tetracyclines in their dosage forms by HPLC using different types of chromatographic stationary phases (RP-C8 and RP-C18)

2021 ◽  
Vol 1 (2) ◽  
pp. 1-10
Keyword(s):  
Analytical Method ◽  
Stationary Phases ◽  
Dosage Forms ◽  
Different Types

scholarly journals Quantification of Fructans in Bioethanol Stillage Based On a Simplified Analytical Method

2021 ◽  
Author(s):  
Andreas Zimmermann ◽  
Martin Kaltschmitt
Keyword(s):  
Analytical Method ◽  
Measurement Errors ◽  
Process Development ◽  
Stationary Phases ◽  
New Approach ◽  
Sample Matrix ◽  
Sample Throughput ◽  
Complex Sample ◽  
Potential Substrate

Abstract Bioethanol stillage, the main by-product of industrial bioethanol production, is a potential substrate for fructans. However, the determination and quantification of fructans in such complex sample matrices is still a challenge for the corresponding analytics to be overcome in order to allow for the identification and utilisation of such unused fructan sources. Especially a possible utilisation or rather the corresponding process development requires appropriate analytics first. Thus, this paper aims to illuminate the basics of fructan quantification in stillage and the corresponding challenges particularly arising with widely used HPLC-RID systems. On this basis, a new approach for fructan quantification is presented based on such HPLC-RID systems allowing for a reliable and especially simple fructan determination in bioethanol stillage for comparably high sample throughput. The developed method performs fructan quantification by determination of fructose and glucose equivalents after a targeted acidic hydrolysis adapted to the respective sample matrix. By means of two different stationary phases, the problem of limited resolution in case of HPLC-RID is overcome and thus measurement errors are reduced. The approach towards the adapted analytical method can be transferred easily to comparable complex sample matrices.

Comparative Study of Methods for the Extraction of Eleven Organophosphorus Pesticide Residues in Rice

1975 ◽  
Vol 58 (6) ◽  
pp. 1286-1293
Author(s):  
Yoichi Aoki ◽  
Mitsuharu Takeda ◽  
Mitsuru Uchiyama
Keyword(s):  
Analytical Method ◽  
Pesticide Residues ◽  
Organophosphorus Pesticides ◽  
Stationary Phases ◽  
Organophosphorus Pesticide ◽  
Extraction Methods ◽  
Rice Samples ◽  
Liquid Chromatographic ◽  
Unpolished Rice

Abstract Several extraction methods are compared for the simultaneous analysis of organophosphorus pesticides in unpolished rice. Four stationary phases were used for the subsequent gas-liquid chromatographic (GLC) determination of the selected pesticides. Using 3 different GLC columns, 11 pesticides were completely separated and identified. The efficiency of the cleanup and the sensitivity of the analytical method were evaluated by using powdered unpolished rice samples fortified with the pesticides and also wheat and dried bean samples. Average recoveries ranged from 74.7% for disulfoton to 97.4% for malathion in unpolished rice and from 68.1% for disulfoton to 108.3% for malathion in other crops. The method described is applicable to the analysis of selected organophosphorus pesticide residues in unpolished rice, wheat, buckwheat, and dried beans.

scholarly journals TLC-densitometric analysis of α-escin in bulk drug substance and in pharmaceutical dosage forms

2015 ◽  
Vol 28 (3) ◽  
pp. 186-191
Author(s):  
Malgorzata Dolowy ◽  
Alina Pyka-Pajak ◽  
Katarzyna Filip ◽  
Joanna Zagrodzka
Keyword(s):  
Sulphuric Acid ◽  
Mobile Phase ◽  
Stationary Phases ◽  
Dosage Forms ◽  
Oral Dosage ◽  
Pharmaceutical Dosage Forms ◽  
Drug Substances ◽  
Subsequent Application ◽  
Bulk Drug

Abstract A quite simple and rapid TLC-densitometric method for the identification of α-escin (Aescin) in bulk drug substances was developed. In so doing, different chromatographic conditions, including various mobile and stationary phases, were tested. A TLC densitometric determination of the examined compound was performed without using visualizing reagent, yet with the use of appropriate dipping reagents, in order to obtain reliable UV-densitometric measurements of α-escin - a substance which has weak chromophore groups. Herein, the application of a mobile phase containing n-butanolacetic acid-water in volume composition 30:7:13, the use of silica gel 60F254 plates with concentrating zone, and subsequent application of 10% sulphuric acid in ethanol or 5% vanillin in methanol/sulphuric acid, respectively, provided the best results in a TLCdensitometric study of α-escin. The described method was successfully employed to identify α-escin in commercial samples that were in an oral dosage form (tablets) and also in the form of gel containing 20 mg of α-escin.

scholarly journals Determination of illegal colorants in grilled meats by liquid chromatography-tandem mass spectrometry

2020 ◽  
Vol 3 (4) ◽  
pp. 23-28
Author(s):  
Huyen Doan Thu ◽  
Thanh Ha Pham Thi ◽  
Ha Nguyen Quang ◽  
Thuy Duong Luong Nguyen ◽  
Van Trinh Viet ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Analytical Method ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Different Types ◽  
Liquid Chromatography Tandem Mass ◽  
Meat Samples

An analytical method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was validated for the simultaneous determination of three illegal colorants including chrysoidine G, para red, and pararosaniline in grilled meat. The meat samples were homogenized and extracted by QuEChERS, and analyzed by LC-MS/MS. Good linearity was obtained in a range of 30 - 1000 µg/L, 5 - 1000 µg/L, and 0.5 - 1000 µg/L  for chrysoidine G, para red, and pararosaniline, respectively. The repeatability and accuracy of the method were adequate with the recoveries ranged from 90% to 98% and RSD% of 5.3 to 10.7% for 3 compounds. The procedure was applied for 49 samples of different types of grilled meat collected from six different areas in Hanoi. Chrysoidine G was detected in 19 samples. It's remarkable that among these positive samples, 6 samples were found negative on homogenized samples, and positive with chrysoidine selected sample with the more intensely colored surface part.

Elemental Impurities Determination by ICP-AES / ICP-MS: A review of Theory, Interpretation of Concentration Limits, Analytical Method Development Challenges and Validation Criterion for Pharmaceutical Dosage Forms

2020 ◽  
Vol 16 (4) ◽  
pp. 392-403
Author(s):  
Lakshmi Narasimha Rao Katakam ◽  
Hassan Y. Aboul-Enein
Keyword(s):  
Analytical Method ◽  
Method Development ◽  
Drug Product ◽  
Dosage Forms ◽  
Drug Substance ◽  
Individual Element ◽  
Pharmaceutical Dosage Forms ◽  
Elemental Impurities ◽  
Icp Ms

: Inductively coupled plasma is a new technique employed for the determination of elemental impurities in pharmaceutical ingredients viz. raw materials, drug substance, and drug product dosage forms. New US FDA and EMA regulations came into effect from Jan 2018 as industry standard requirements for the determination of inorganic elemental impurities using ICP-OES/AES or ICP-MS analytical techniques. The method development was optimized for the determination of the listed elements as per USP <232> <233> elemental impurities-limits and procedures. It also demonstrates the validation of the method and verification/transfer of the method which also provides an insight into the presence of free elemental atomics of the gaseous form of the sample (drug substance, drug product or excipients), thus helping in determining the concentration of the element of interest. Also, the regulatory guidance is very general and does not explain the sample specifications for the individual element concentrations. Thus, this review emphasizes the routine instrumental maintenance, analytical method development challenges, trends in the performance of analytical method validation and verification/ transfer activities of the various pharmaceutical dosage forms outlined with acceptance criterion.

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