Development and validation of qualitative screening, quantitative determination and post-targeted pesticide analysis in tropical fruits and vegetables by LC-HRMS

2021 ◽  
pp. 130714
Author(s):  
Iván Mauricio Huérfano Barco ◽  
Julio César España Amórtegui ◽  
Jairo Arturo Guerrero Dallos
Keyword(s):  
Quantitative Determination ◽  
Fruits And Vegetables ◽  
Pesticide Analysis ◽  
Tropical Fruits ◽  
Development And Validation

Development and Validation of HPLC/UV-Spectrophotometric Procedures for Metronidazole Quantitative Determination

2018 ◽  
Vol 9 (3) ◽  
Author(s):  
Klimenko Lina Yu ◽  
Shkarlat Galyna L ◽  
Shovkova Zoia V ◽  
Yaremenko Vitaliy D ◽  
Shpychak Oleg S
Keyword(s):  
Quantitative Determination ◽  
Sodium Hydroxide Solution ◽  
Gradient Elution ◽  
Calibration Model ◽  
Column Temperature ◽  
Medical Laboratories ◽  
Accuracy And Precision ◽  
Development And Validation ◽  
Gradient Elution Mode ◽  
Potential Object

Metronidazole is the most popular representative of antiprotozoal medicines from the group of 5-nitroimidazoles. Metronidazole blocks the enzymes of alcohol dehydrogenase and acetaldehyde dehydrogenase, therefore when its joint taking with alcohol it is observed the strong intoxication syndrome and fatal poisonings too. Therefore metronidazole can be a potential object of chemical toxicological investigations. The purpose of our paper is to develop HPLC/UV-procedure of metronidazole quantification with application of the system of HPLC-analyzer MiLiChrome® A-0230 implemented in practice of forensic medical laboratories in Russia and Ukraine and carry out step-by-step validation of the developed procedure. Chromatographic conditions: Eluent A (0.2 M LiClO4 – 0.005 M HClO4) and Eluent B (acetonitrile) wereused as the mobile phase components; HPLC microcolumn Ø2×75 mm and ProntoSIL 120-5-C18 AQ, 5 μm were used as an analytical column; temperature was 40°С; flow rate was 100 μl/min; gradient elution mode was from 5% to 100% Eluent B for 40 min, then 100% Eluent B for 3 min; detection was performed at 277 nm. Retention time for metronidazole is 5.95 min. Since metronidazole is easy soluble and stable enough in the solutions of diluted alkalis 0.001 M sodium hydroxide solution has been proposed for preparation of the solutions in developing HPLC/UV-procedure of metronidazole quantification. Validation of the procedure has been carried out in the variants of the method of calibration curve and method of standard by such parameters as in process stability, linearity/calibration model, accuracy and precision within 3 different analytical runs using different batches of reagents and different glassware; experiments have been performed by three different analysts. New procedure of metronidazole quantitative determination by the method of HPLC/UV has been developed. Its validation has been carried out and acceptability for application has been shown.

Multi-residue pesticide analysis in fruits and vegetables by liquid chromatography–time-of-flight mass spectrometry

2005 ◽  
Vol 1082 (1) ◽  
pp. 81-90 ◽  
Author(s):  
Imma Ferrer ◽  
Juan F. García-Reyes ◽  
Milagros Mezcua ◽  
E. Michael Thurman ◽  
Amadeo R. Fernández-Alba
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Fruits And Vegetables ◽  
Time Of Flight ◽  
Pesticide Analysis ◽  
Flight Mass Spectrometry

scholarly journals Development and Validation of an UHPLC Method for Ostarine Determination in Dietary Supplements

2019 ◽  
Vol 65 (2) ◽  
pp. 49-54
Author(s):  
Amalia Miklos ◽  
Amelia Tero-Vescan ◽  
Lénárd Farczádi ◽  
Daniela-Lucia Muntean
Keyword(s):  
Quantitative Determination ◽  
Dietary Supplements ◽  
Low Cost ◽  
Reversed Phase ◽  
European Pharmacopoeia ◽  
Average Mass ◽  
7Th Edition ◽  
Development And Validation ◽  
Mg Content

AbstractObjective: The purpose of this study was to develop a low-cost, yet sensitive and precise UHPLC method for the quantitative determination of ostarine from dietary supplements (DS) for athletes. The analytical performance of the method was verified on a DS legally acquired from a specialized website for athletes. The uniformity of mass and content of the ostarine DS was also verified.Methods: For the quantitative determination of ostarine a UHPLC method was developed and validated. The separation was performed using a reversed-phase C18 column, using a mixture of 75% methanol: 25% formic acid 0.1% in isocratic elution, at a flow rate of 0.5 ml/min. The uniformity of mass and content of DS was performed following the methodology described in the European Pharmacopoeia 7th Edition.Results: The validated method was specific and linear on the concentration range of 1-25 µg/ml and was precise and accurate at all concentration levels, according to the official guidelines for validating analytical methods. An average mass of 510 mg content was obtained for the ostarine capsules, with an RSD of 2.41%. Regarding the uniformity of the content, an average of 4.65 mg ostarine/capsule was obtained with an RSD of 1.05%.Conclusions: The developed UHPLC method was suitable, rapid, sensitive and allowed quantitative determination of active substance content in a DS with ostarine (92.91% ostarine/capsule from 5 mg ostarine/capsule declared by the manufacturer).

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