scholarly journals Method Validation of Drug Quantification Poster

2020 ◽  
Author(s):  
Fathy Atia Mohamed Atia ◽  
Ahmad Ali Ahmadi ◽  
Mohammed AlSafran
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Detection Limit ◽  
Flow Rate ◽  
Calibration Curve ◽  
Method Detection Limit ◽  
Quantification Limit ◽  
Accuracy And Precision ◽  
Organic Extraction ◽  
Validation Criteria

A lowest detection limit with straight linearity was obtained by developing a method to analyze Phenacetin (Phe) in both aqueous and organic extraction by using Liquid chromatography Triple Quoadrpole mass with electrospray ionization (LCMSMS/ESI). The validation of the developed method was carried out according to ICH Harmonized Tripartite guideline. Validation criteria obtained were; the method detection limit MDL is 0.089 ng/ml, method quantification limit MQL is 0.19 ng/ml while the calibration curve linear from 0.1 to 1000 ng/mL with correlation coefficient R2 is 0.9994, Accuracy and precision up to 97% and the repeatability inter and intraday for six replicates of three concentration with RSD 2.1%. Separation occurred using Nova Pack C18 4 um, 150 x 3.9 mm column, using acetonitrile: 0.1% Formic acid 60:40% (v:v) at flow rate 1ml/min. the detector was triple quad mass spectrometry at multi-reaction mode MRM to detect parent mass 180.1 at frag 97 to transition fragments 110 and 138 at collision voltages 16 and 12 respectively.

scholarly journals Simultaneous Determination of Levocetirizine and Pseudoephedrine in Dog Plasma by Liquid Chromatography-Mass Spectrometry in the Presence of Dextrocetirizine

2012 ◽  
Vol 15 (4) ◽  
pp. 519 ◽  
Author(s):  
Jae Kuk Ryu ◽  
Sun Dong Yoo
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Oral Administration ◽  
Mobile Phase ◽  
Internal Standard ◽  
Liquid Chromatography Mass Spectrometry ◽  
Chiral Column ◽  
Accuracy And Precision ◽  
Dog Plasma

Purpose. This study describes the development of a rapid and sensitive LC-ESI-MS assay for simultaneous enantioselective determination of levocetirizine and pseudoephedrine in dog plasma in the presence of dextrocetirizine. Methods. Separations were achieved on an Ultron ES-OVM chiral column using the mobile phase consisting of 10 mM aqueous NH4OAc (pH 6.6) and acetonitrile (9:1 v/v). Results. The retention times of pseudoephedrine, dextrocetirizine, levocetirizine and diazepam (internal standard) were 5.2, 8.3, 9.6 and 11.6 min, respectively, and the total run time was less than 15 min. The assay was validated to demonstrate the linearity, accuracy and precision, recovery and stability. The calibration curves were linear over the concentration range from 1 – 200 ng/mL for levocetirizine and from 5 – 1000 ng/mL for pseudoephedrine. Conclusions. The developed assay was successfully applied to a pharmacokinetic study after oral administration of the racemic cetirizine (0.5 mg/kg, or 0.25 mg/kg as levocetirizine) and pseudoephedrine (12 mg/kg) in the dog. This article is open to POST-PUBLICATION REVIEW. Registered readers (see “For Readers”) may comment by clicking on ABSTRACT on the issue’s contents page.

scholarly journals Validation of High Performance Liquid Chromatography Methods for Determination of Meloxicam and Tenoxicam from Transdermal Therapeutic Systems

2017 ◽  
Vol 63 (4) ◽  
pp. 178-182 ◽  
Author(s):  
Paula Antonoaea ◽  
Anca Gabriela Cârje ◽  
Adriana Ciurba ◽  
Nicoleta Todoran ◽  
Alexandru Robert Vlad ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Detection Limit ◽  
High Performance ◽  
Hydroxypropyl Methylcellulose ◽  
Active Pharmaceutical Ingredient ◽  
Performance Criteria ◽  
Quantification Limit ◽  
Transdermal Patches ◽  
Evaporation Technique

AbstractObjective: The aim of this study was to develop and validate two HPLC methods for the quantification of meloxicam and tenoxicam from transdermal therapeutic systems.Methods: Based on 1.0% hydroxypropyl methylcellulose 15000, transdermal patches containing meloxicam or tenoxicam were prepared by solvent evaporation technique. Analytical performances of the HPLC methods for the quantification of meloxicam and tenoxicam from such systems were assessed in terms of specificity, linearity, detection limit, quantification limit, recovery and precision.Results and discussion: The linearity of the method was assessed through a calibration curve in the 1.0 - 75.0 μg∙mL−1concentration range, with a regression coefficient higher than 0.999. The detection limit and the quantification limit were found to be 0.46 μg∙mL−1and 1.39 μg∙mL−1, for meloxicam; and 0.88 μg∙mL−1, respectively 2.64 μg∙mL−1for tenoxicam. According to the European Pharmacopeia 5.0 the mean recovery was found to be between 75% and 125%. As performance criteria for precision was used the RSD% which were lower than 2.0% for both methods.Conclusions: The proposed liquid chromatography methods provide selective, linear and precise results for the quantification of meloxicam and tenoxicam from transdermal therapeutic systems. The presence of a single peak in the chromatograms of the analyzed transdermal patches with meloxicam or tenoxicam, certify the successful determination of the active pharmaceutical ingredient in the prepared patches.

scholarly journals Capillary photoionization: interface for low flow rate liquid chromatography-mass spectrometry

The Analyst ◽  
2019 ◽  
Vol 144 (9) ◽  
pp. 2867-2871 ◽  
Author(s):  
Päivi Pöhö ◽  
Anu Vaikkinen ◽  
Markus Haapala ◽  
Petri Kylli ◽  
Risto Kostiainen
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Mass Spectrometer ◽  
Flow Rate ◽  
Low Flow ◽  
Liquid Chromatography Mass Spectrometry ◽  
Liquid Chromatograph ◽  
First Report ◽  
Chromatography Mass Spectrometry ◽  
Low Flow Rate

The first report on capillary photoionization interfacing a liquid chromatograph and mass spectrometer.

scholarly journals Determination of Tributyltin in Seafood Based on Magnetic Molecularly Imprinted Polymers Coupled with High-Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

2017 ◽  
Vol 2017 ◽  
pp. 1-11
Author(s):  
Hua Yang ◽  
Huien Zhang ◽  
Xiao Yan Zhu ◽  
Shi Da Chen ◽  
Lijun Liu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Detection Limit ◽  
Molecular Imprinting ◽  
Inductively Coupled Plasma ◽  
High Performance ◽  
Linear Range ◽  
Inductively Coupled ◽  
Plasma Mass Spectrometry

In this study, Fe3O4 was adopted as a carrier for surface molecular imprinting with two-stage polymerization. First, the functional monomer (methacrylic acid, MAA) was modified on the surface of Fe3O4, which was then polymerized with the template molecule (tributyltin, TBT), cross linking agent (ethylene glycol dimethacrylate, EGDMA), and porogen (acetonitrile), hereby successfully preparing Fe3O4@MIPs prone to specifically identify TBT. The physical properties of Fe3O4@MIPs were then characterized, and adsorption and selection capacities were also assessed. Compared with conventional imprinting polymers, this magnetic molecular imprinting polymer (MIP) displayed significantly increased and more specific adsorption. Meanwhile, its pretreatment was simpler and faster due to magnetic separation characteristics. Using magnetic MIPs as adsorbents for enrichment and separation, detection limit, recovery rate, and linear range were 1.0 ng g−1, 79.74–95.72%, and 5 ng g−1~1000 ng g−1, respectively, for a number of seafood samples. High-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) was used to analyze Tegillarca granosa, mussels, large yellow croaker, and other specimens, with recovery rates of 79.74–95.72% and RSD of 1.3%–4.7%. Overall, this method has a shorter total analysis time, lower detection limit, and wider linear range and can be more effectively applied to determine MAA in seawater and seafood.

scholarly journals Comparison of two clean up techniques in isolation of ochratoxin A from red wine

2010 ◽  
Vol 28 (No. 3) ◽  
pp. 233-241 ◽  
Author(s):  
E. Belajová ◽  
D. Rauová
Keyword(s):  
Acetic Acid ◽  
Liquid Chromatography ◽  
Detection Limit ◽  
Ochratoxin A ◽  
Red Wine ◽  
Solid Phase ◽  
Phase Extraction ◽  
Immunoaffinity Column ◽  
Experimental Conditions ◽  
Quantification Limit

Two procedures for the extraction of ochratoxin A (OTA) from red wine &ndash; the reference clean up procedure using specific immunoaffinity column (IAC), and solid phase extraction (SPE) in which an active carbon was employed, was compared. In SPE procedure, various mixtures of dichloromethane (D), toluene (T), acetonitrile (AC), methanol (M), and acetic acid (A) were used as OTA desorption agents. Two types of SPE carbonaceous columns were tested &ndash; commercial SPE columns (Supelclean<sup>TM</sup> Envi-Carb) with a nonporous graphitised carbon, and SPE columns prepared in our laboratory (further specified as Lab-Carb) that were filled with a micro particular granular carbon. OTA was extracted from spiked red wine by the use of both carbonaceous columns. The highest OTA mean recovery calculated in relation to the reference IAC procedure was 98.5%, using the Lab-Carb adsorbent and acetonitrile + toluene, 3 + 1 (v + v) as the elution mixture (OTA spike levels of 0.2 &micro;g/l). Using the elution mixture of dichloromethane + methanol, 9 + 1 (v + v), the relative recoveries of 76.4% and 82.9% were reached at the OTA spike levels of 0.2 &micro;g/l and 1.9 &micro;g/l, respectively. The application of Envi-Carb adsorbent generally resulted in a very poor OTA recovery under the experimental conditions used (less than 50%). OTA was detected by liquid chromatography with fluorescence detection (LC-FLD) providing the detection limit of 0.011 &micro;g/l and the quantification limit of 0.033 &micro;g/l. &nbsp;

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