Search results for "Method validation"

Algorithms and software for biological multiscale image analysis

2013

Mycotoxin Analysis of Human Urine by LC-MS/MS: A Comparative Extraction Study

2017

The lower mycotoxin levels detected in urine make the development of sensitive and accurate analytical methods essential. Three extraction methods, namely salting-out liquid–liquid extraction (SALLE), miniQuEChERS (quick, easy, cheap, effective, rugged, and safe), and dispersive liquid–liquid microextraction (DLLME), were evaluated and compared based on analytical parameters for the quantitative LC-MS/MS measurement of 11 mycotoxins (AFB1, AFB2, AFG1, AFG2, OTA, ZEA, BEA, EN A, EN B, EN A1 and EN B1) in human urine. DLLME was selected as the most appropriate methodology, as it produced better validation results for recovery (79–113%), reproducibility (RSDs < 12%), and repeatability (RSDs…

Liquid chromatography in pharmaceutical analytics

2017

Tutkielmassa perehdytään nestekromatografian käyttöön lääkeaineanalytiikassa. Korkean erotuskyvyn nestekromatografia (HPLC) on suosittu menetelmä lääkeaineiden analysoinneissa, esimerkiksi pitoisuuksien tai epäpuhtauksien määrityksissä. HPLC-menetelmät voidaan luokitella useisiin alalajeihin ja käänteisfaasinestekromatografia (RP-HPLC) on niistä suosituin lääkeaineanalytiikassa. Tässä kirjallisuuskatsauksessa käsitellään erityisesti nopeaa nestekromatografiaa. Analyysimenetelmiä voidaan nopeuttaa sopivan kolonnin avulla. Tavanomainen HPLC-ajo on mahdollista toteuttaa lyhyemmässä ajassa käyttämällä lyhyttä kolonnia tai kolonnia, jossa partikkelikoko on pieni. Kuitenkin tehokkain tapa on käyt…

Development of fast analysis methods for extractives in papermaking process waters

2011

A fast analysis method with an online sample enrichment technique for the analysis of resin and fatty acids present in papermaking process waters was developed. This method was based on atmospheric pressure chemical ionization (APCI) and mass spectrometry (MS) for the detection of [M-H]- ions of compounds of interest. The method was applied to the control of the most prevalent resin (dehydroabietic and abietic) and fatty (palmitic, stearic, oleic, and linolenic) acid levels in papermaking process waters. Continuous data on these acids are of practical importance when predicting possible deposit-derived problems in the paper machine. The first part of the study was focused on the development…

Are analysts doing method validation in liquid chromatography?

2014

International audience; Method validation is being applied in the reported analytical methods for decades. Even before this protocol was defined, authors already somehow validated their methods without full awareness. They wished to assure the quality of their work. Validation is an applied approach to verify that a method is suitable and rugged enough to function as a quality control tool in different locations and times. The performance parameters and statistical protocols followed throughout a validation study vary with the source of guidelines. Before single laboratory validation, an analytical method should be fully developed and optimized. The purpose of the validation is to confirm p…

Analysis of enniatins and beauvericin by LC-MS/MS in wheat-based products

2017

Due to the matrix complexity for wheat-based products, a comparative study of different rapid extraction procedures was performed for the extraction of enniatins (ENA, ENA1, ENB, ENB1) and beauvericin in flour, pasta, breakfast cereals, and biscuits. Three different approaches were studied during the extraction and purification steps (shaker, Ultra-Turrax, and QuEChERS) for each matrix. Liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) with electrospray source working in a positive mode was used. For the analysis of the five mycotoxins, the three methods were tested in terms of recovery, matrix effect, and sensibility, concluding that Ultra-Turrax extraction was the most …

Analysis of basic drugs by liquid chromatography with environmentally friendly mobile phases in pharmaceutical formulations

2017

Abstract Basic drugs are positively charged in the usual working pH (2–8) in reversed-phase liquid chromatography. This gives rise to a strong association with the residual ionized silanols in conventional silica-based stationary phases, which is translated in poor peak shape and high consumption of organic solvent to get appropriate retention times. Micellar mobile phases containing surfactants give rise to modified stationary phases, where silanols are masked, improving the peak shape. However, mobile phases containing the anionic surfactant sodium dodecyl sulfate (SDS) require a small amount of organic solvent to conveniently decrease the retention of cationic analytes. An alternative is…